CN103554936A - Asphalt-mineral composite material prepared by utilizing thickened oil sludge and preparation method thereof - Google Patents
Asphalt-mineral composite material prepared by utilizing thickened oil sludge and preparation method thereof Download PDFInfo
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Abstract
The invention provides a method for preparing an asphalt-mineral composite material by utilizing thickened oil sludge. The method comprises the following steps: after mixing the thickened oil sludge with a softening point conditioning agent, carrying out high temperature melting; after stopping heating, adding a hard brittle material, and melting the hard brittle material by utilizing residual temperature of the mixture of the thickened oil sludge and the softening point conditioning agent; after stirring into an uniform fluid, carrying out sudden cooling, and then carrying out steps of drying, crushing and the like to prepare the asphalt-mineral composite material. The method provided by the invention realizes the resource utilization on the harmless basis of the thickened oil sludge, and can create certain economic values while reducing the environmental pollution; the invention also provides the asphalt-mineral composite material prepared by adopting the method, and the obtained product can be widely applied to various fields of waterproof roll material, road asphalt, waste rubber powder regeneration, oil field chemicals and the like without secondary pollution.
Description
Technical field
The present invention relates to the recycling field of thick oil sludge, particularly viscous oil recovery and containing the innoxious and recycling of the thick oil sludge producing in condensed oil sewage treating processes in a kind of petroleum industry.
Background technology
Thick oil sludge is mainly derived from viscous crude field Oil extraction process and the oily sludge producing in oil field gathering and transportation process, mainly comprises the residual active sludge after oil trap bed mud, tank bed mud, scum bottom sludge and the sewage biochemical treatment that sewage treatment system of oilfield produces.In thick oil sludge, resin and asphalt component concentration is high, also higher in conjunction with the clay mineral content existing with colloidal form, this two classes material is the main nonaqueous component of thick oil sludge, its viscosity is large, density is large, is difficult for dehydration, and conventional process for treating oil-containing sludge, as loss on drying, solvent extraction, stripping, drip washing, solvent extraction-ultrasonic separation, burning, oxidation, biological restoration, microbial de-emulsification etc., be not suitable for processing thick oil sludge.
Thick oil sludge complicated component, belongs to heterogeneous system, wherein contains a large amount of aging crude oil, wax, bituminous matter, colloid and suspended solid, bacterium, salt, sour gas, corrosion product and a small amount of heavy metal, oxygenant and salt etc.In simultaneously viscous oil recovery and condensed oil sewage treating processes, added the water treatment agents such as a large amount of degreasers, organic and inorganic flocculating agent, inhibiter, Scale inhibitors, sterilant, wherein solid phase be take clay class dirt as main; Liquid phase part is mainly the sufficient emulsion of emulsification, and form is oil-in-water (O/W) or water-in-oil (W/O).Because composition and the character of thick oil sludge are complicated, intractability is large, there is again low nutrition simultaneously, low-permeability, the features such as nutrition and oxygen skewness, therefore its poor stability, easy corrupt and generation stench, benzene homologues wherein particularly, phenol, it is very harmful that pyrenes etc. have the material of foul smell and toxicity, the organic danger wastes of HW08 class that belongs to regulation in China < < Hazardous Waste List > > of country (version in 2008), serious threat is to the people's life and health.
Tradition disposal of oily sludge pattern mainly comprises following several: 1. solidify, adopt the materials such as cement that thick oil sludge is solidified to rear landfill, reduce the harm to environment; 2. centrifugal, for the high greasy filth of solids content, although after this processes in greasy filth oleaginousness still very high, can recovery part crude oil; 3. dewater, burn, the method solves comparatively up hill and dale greasy filth and pollutes, but exists equipment power consumption high, the phenomenons such as crude resources waste, and be difficult to the long-time running of the equipment that guarantees.
The technology that recent domestic relates to while processing oily sludge mainly comprises sludge pretreatment, thermal treatment, solvent extraction processing, biological treatment and comprehensive utilization etc.For example US Patent No. Pat.6673231 is used pyrogen oil flushing tank bed mud, then distills processing, and its treatment effect is good, but cost is expensive, and energy consumption is large.Chinese patent CN200710145460 disclosure of the invention a kind of process for treating oil-containing sludge, comprise concentration, the steps such as flocculation-centrifuge dehydration and drying and other treatment, its technological process is loaded down with trivial details, length consuming time, though realized environmental benefit, does not have economic benefit.Chinese patent CN201110080196 discloses oily sludge and has focused on the treatment process with recycling, the method obtains mud cake and sewage through multistep dehydration separation, as moulded coal mixed material, utilize, but the round circulation step of the method is too much, installation cost is too high.World patent WO2011074007 and US Patent No. Pat.2008264856 carry out bioreediation to oily sludge respectively, utilize microorganism to carry out oil removal treatment, but cost are higher, and process is wayward.World patent WO2009028518, Chinese patent CN201338974 and US Patent No. Pat.20060012970 respectively research and design the treatment unit of several different oily sludges, this class methods initial outlay is larger, ageing not strong, treatment effect is unstable, because of oily different.
Chinese patent CN101045600A provides a kind for the treatment of process of thick oil sludge bituminous grouting, technical scheme comprises: (1) gets the thick oil sludge of oil removal after pretreatment, flotation generation, be positioned in batch type reactor, under mechanical stirring, heat up and heat, open vacuum pump simultaneously, under reduced pressure distill, drawing-off water steam, oil gas, then condensation is reclaimed; (2) when temperature reaches 330～370 ℃, keep this temperature until do not distillate oil gas in still and stop heating, take out surplus materials in still, cooling forming obtains bituminous grouting product.But there is following several respects defect in above-mentioned technique: 1. the moisture in thick oil sludge, oil content and solid have formed stable emulsified state, under low temperature, be difficult for distillation, in the course of processing, temperature need to be up to 370 ℃, therefore, the high energy consumption that pyroreaction causes can cause cost high, meanwhile, high temperature process also can cause will greatly reducing as the bounding force of the main performance of pitch, thus grievous injury asphalt quality; 2. aforesaid method gained bituminous grouting products collection efficiency is low, less than 30%; 3. because obtained bituminous grouting product output is little, quality is low, its economy is unsatisfactory.
Summary of the invention
For solving the problems of the technologies described above, the inventor is through research with keen determination, found that, utilize the colloid of high-content in thick oil sludge and bituminous matter component and contained clay mineral colloid can prepare a kind of pitch-mineral composite with widespread use field and using value, to realize the comprehensive utilization of waste resource, it consists of thick oil sludge, softening temperature conditioning agent and hard brittle material, it makes pitch-mineral composite after blended melting, quenching and pulverizing, particularly, the invention provides following several respects:
First aspect, the invention provides a kind of pitch-mineral composite that utilizes thick oil sludge to prepare, and it is characterized in that, by the composition that comprises following weight proportion, is made:
Thick oil sludge: 40～80 parts;
Softening temperature conditioning agent: 10～30 parts;
Hard brittle material: 5～20 parts,
Wherein,
Described thick oil sludge is the mud containing viscous crude of the outer row of oily water treatment joint station in petroleum industry viscous oil recovery process;
Described hard brittle material is selected from: oil soluble petroleum resin, brown coal or its mixture;
Described softening temperature conditioning agent is selected from: the mixture that one or more arbitrary proportions in Gum Rosin natural or synthetic, dehydration fusel, high softening point bitumen, biological carbon, xylogen and humic acids form, wherein,
Described high softening point bitumen is softening temperature higher than the pitch of 150 ℃;
The multiporous biological carbon of described biological carbon for being processed by organic by-products such as animal excrement, animal bone, plant roots and stems, wood chip or Wheat Straws;
The product that described dehydration fusel obtains after dehydration reaction for be greater than 2 aliphatics alcohols by carbonatoms;
Described pitch-mineral composite is prepared and is obtained by following steps:
(1) by above-mentioned weight proportion, take thick oil sludge and softening temperature conditioning agent evenly mixes, after mixing, under melt temperature is the condition of 80～200 ℃, carry out melting;
(2) in step (1), mixture reaches after molten state, stops heating, adds immediately hard brittle material, utilizes the remaining temperature of mixture that hard brittle material is melted, and is stirred to be in normal-temperature water, to carry out after uniform fluid suddenly coolingly, obtains matrix material body;
(3) the matrix material body through obtaining in step (2) is carried out to seasoning, being ground into particle diameter after to be dried is 60～100 object powder granules.
Second aspect, the invention provides above-mentioned a kind of pitch-mineral composite that utilizes thick oil sludge to prepare, and it is characterized in that, comprises the composition of following weight proportion:
Thick oil sludge: 55～75 parts;
Softening temperature conditioning agent: 15～22 parts;
Hard brittle material: 10～15 parts;
Described in step (1), melt temperature is 100～150 ℃;
Described in step (3), crushing process carries out in air blast cooling crush machine;
Described high softening point bitumen is softening temperature higher than the pitch of 180 ℃.
The third aspect, the invention provides above-mentioned a kind of pitch-mineral composite that utilizes thick oil sludge to prepare, it is characterized in that, described high softening point bitumen is the pitch of 190～260 ℃ of softening temperatures, is selected from: originate from the mixture that one or more arbitrary proportions in the rock asphalt on the ground such as Xinjiang, Sichuan, Iran form.
Fourth aspect, the invention provides a kind of method of utilizing thick oil sludge to prepare pitch-mineral composite, it is characterized in that, comprises the following steps:
(1) take thick oil sludge and softening temperature conditioning agent evenly mixes, after mixing, under melt temperature is the condition of 80～200 ℃, carry out melting;
(2) in step (1), mixture reaches after molten state, stops heating, adds immediately hard brittle material, utilizes the remaining temperature of mixture that hard brittle material is melted, and is stirred to be in normal-temperature water, to carry out after uniform fluid suddenly coolingly, obtains matrix material body;
(3) the matrix material body through obtaining in step (2) is carried out to seasoning, being ground into particle diameter after to be dried is 60～100 object powder granules,
Wherein,
Described thick oil sludge is the heavy crude oily sludge that contains that in petroleum industry viscous oil recovery process, oily water treatment joint station is arranged outward;
Described hard brittle material is selected from: oil soluble petroleum resin, brown coal or its mixture;
Described softening temperature conditioning agent is selected from: the mixture that one or more arbitrary proportions in Gum Rosin natural or synthetic, dehydration fusel, high softening point bitumen, biological carbon, xylogen and humic acids form, wherein,
Described high softening point bitumen is softening temperature higher than the pitch of 150 ℃;
The multiporous biological carbon of described biological carbon for being processed by organic by-products such as animal excrement, animal bone, plant roots and stems, wood chip or Wheat Straws;
Described dehydration fusel is, by carbonatoms, is greater than the product that two aliphatics alcohols obtains after dehydration reaction.
The 5th aspect, the invention provides a kind of above-mentioned method of utilizing thick oil sludge to prepare pitch-mineral composite, it is characterized in that,
Described in step (1), melt temperature is 100～150 ℃;
Described in step (3), crushing process carries out in air blast cooling crush machine;
Described high softening point bitumen is softening temperature higher than the pitch of 180 ℃.
The 6th aspect, the invention provides a kind of above-mentioned method of utilizing thick oil sludge to prepare pitch-mineral composite, it is characterized in that, described high softening point bitumen is the pitch of 190～260 ℃ of softening temperatures, is selected from: originate from the mixture that one or more arbitrary proportions in the rock asphalt on the ground such as Xinjiang, Sichuan, Iran form.
The 7th aspect, the invention provides a kind of above-mentioned method of utilizing thick oil sludge to prepare pitch-mineral composite, it is characterized in that, comprises the composition of following weight proportion:
Thick oil sludge: 40～80 parts;
Softening temperature conditioning agent: 10～30 parts;
Hard brittle material: 5～20 parts.
Eight aspect, the invention provides a kind of above-mentioned method of utilizing thick oil sludge to prepare pitch-mineral composite, it is characterized in that, comprises the composition of following weight proportion:
Thick oil sludge: 55～75 parts;
Softening temperature conditioning agent: 15～22 parts;
Hard brittle material: 10～15 parts.
The 9th aspect, the invention provides and a kind ofly utilize pitch-mineral composite prepared by thick oil sludge for the purposes of waterproof roll, bitumen for road use and waste rubber regeneration.
The tenth aspect, the invention provides and a kind ofly utilize pitch-mineral composite prepared by thick oil sludge for the purposes of petroleum drilling anti-sloughing agent.
According to a kind of pitch mineral composite that utilizes thick oil sludge to prepare the method for pitch-mineral composite and prepare by the method provided by the invention, there is following beneficial effect:
(1) method provided by the invention, can effectively utilize viscous oil recovery in petroleum industry and containing the thick oil sludge producing in condensed oil sewage treating processes, prepare the product with practical value, realizes the harmless treatment of hazardous and noxious substances, and turns waste into wealth;
(2) compare with traditional treatment method, method provided by the invention, for processing thick oil sludge, to have production technique simple, implement convenient and easy, practical, can large-scale promotion to oil production industry;
(3) the inventive method waste utilization rate is high, realizes recycling and produce on innoxious basis, creates certain economic value when reducing environmental pollution;
(4) pitch-mineral composite of preparing according to method provided by the invention approximately contains 2/3rds the oil soluble hydrocarbons such as resin and asphalt, containing 1/3rd ultra tiny inorganic mineral powders, can be widely used in waterproof roll, bitumen for road use, waste rubber regeneration and petroleum drilling anti-sloughing agent etc.;
(5) thick oil sludge is prepared into the pitch-mineral composite having compared with high added value, avoided by greasy filth separately or mixes with coal and be used as the burning of fuel low value, and the meeting of having avoided producing in combustion processes causes the toxic and harmful that contains dioxin of serious environmental pollution.
Embodiment
Further explain and describe by the following examples content of the present invention.But the embodiment providing should not be understood to protection domain of the present invention to be construed as limiting.
The invention provides a kind of pitch-mineral composite that utilizes thick oil sludge to prepare, it comprises the composition of following weight proportion:
Thick oil sludge: 40～80 parts;
Softening temperature conditioning agent: 10～30 parts;
Hard brittle material: 5～20 parts,
Preferably, the composition that comprises following weight proportion:
Thick oil sludge: 55～75 parts;
Softening temperature conditioning agent: 15～22 parts;
Hard brittle material: 10～15 parts.
Wherein,
Described thick oil sludge is the mud containing viscous crude of the outer row of oily water treatment joint station in petroleum industry viscous oil recovery process;
Described hard brittle material is selected from: oil soluble petroleum resin, for example, No. 10 oil-soluble resins, No. 16 oil-soluble resins, but described oil-soluble resin is not only in cited oil-soluble resin example; Brown coal or its mixture.In preparing pitch-mineral composite process, add hard brittle material, can make prepared pitch-mineral composite can be ground into powder body material easy to use by air-cooled pulverizer at normal temperatures.
Described softening temperature conditioning agent is selected from: the mixture that one or more arbitrary proportions in Gum Rosin natural or synthetic, dehydration fusel, high softening point bitumen, biological carbon, xylogen and humic acids form.
There is the solid composite material characteristic that pitch-mineral composite that the thick oil sludge of high softening-point prepares can present class sapropelitic at normal temperatures, pitch-mineral composite that the thick oil sludge of low softening point is prepared is without this characteristic, yet, as in the thick oil sludge of raw material, there is the resin and asphalt component that a large amount of softening temperatures is lower in the present invention, therefore need to add high softening-point material to heighten the softening temperature of thick oil sludge, thereby prepare required pitch-mineral composite, in addition, because the softening temperature of thick oil sludge is lower, in high-temperature fusion process, easily there is the unfavorable side reactions such as carburizing reagent, for avoiding the generation of this type of side reaction, in melting process, add softening temperature conditioning agent, thereby improve the softening temperature of thick oil sludge.The high softening point bitumen that the present invention selects is softening temperature higher than the pitch of 150 ℃, and preferably higher than 180 ℃, preferred softening temperature is 190～260 ℃.
Biological carbon be a kind of organic carbon of fragility, in thick oil sludge, add biological carbon to be both conducive to improve the softening temperature of prepared pitch-mineral composite, also be conducive to increase the fragility of prepared pitch-mineral composite, thereby be convenient to the pulverizing of follow-up pitch-mineral composite.The multiporous biological carbon of the preferred biological carbon of the present invention for being processed by organic by-products such as animal excrement, animal bone, plant roots and stems, wood chip or Wheat Straws.
Dehydration fusel is a kind of polyvalent alcohol mixing by bio-alcohol industrial by-products, and its main component is dibasic alcohol, trivalent alcohol and low-molecular(weight)polymer thereof.Under hot conditions, in fusel contained abundant hydroxyl and the generation esterifications such as carboxyl contained in colloid, bituminous matter, amido and (or) cross-linking chemistry reacts, generation has the more netted condensed ring macromole of high molecular, this condensed ring macromole can strengthen colloid, bitum cementability and toughness, improve the visco-elasticity of prepared matrix material, make it really there is the viscous-elastic behaviour of class sapropelitic.The product that the dehydration fusel that the present invention selects obtains after dehydration reaction for be greater than 2 aliphatics alcohols by carbonatoms, the mixture for example mainly being formed by ethylene glycol, propylene glycol, butyleneglycol, glycerol and oligopolymer thereof, but be not limited to cited dehydration fusel example.
The invention provides a kind of method of utilizing thick oil sludge to prepare pitch-mineral composite, particularly, comprise the following steps:
(1) take thick oil sludge and softening temperature conditioning agent evenly mixes, after mixing, under melt temperature is the condition of 80～200 ℃, carry out melting;
(2) in step (1), mixture reaches after molten state, stops heating, adds immediately hard brittle material, utilizes the remaining temperature of mixture that hard brittle material is melted, and is stirred to be in normal-temperature water, to carry out after uniform fluid suddenly coolingly, obtains matrix material body;
(3) the matrix material body through obtaining in step (2) is carried out to seasoning, being ground into particle diameter after to be dried is 60～100 object powder granules.
Thick oil sludge is the waste that petroleum industry produces in viscous oil recovery, it under normal temperature, is solid-state or semi-solid state, wherein contain a large amount of resin and asphalt materials, there is zero pour high, viscosity is large, the features such as the large and profit density difference of density is little, when temperature is at it more than fusing point, in the time of more than 80 ℃, can with the mutual melting of softening temperature conditioning agent, form even phase mixture, and hard brittle material is selected from oil soluble petroleum resin, brown coal or its mixture, its fusing point is low compared with thick oil sludge and softening temperature conditioning agent, therefore can plant after component melts mixes and add hard brittle material at the first two, rely on its waste heat can realize the melting of hard brittle material, thereby save energy cost, yet melt temperature is unsuitable too high, when temperature is during higher than 200 ℃, can there is carburizing reagent in thick oil sludge, thereby cause the reduction of composite products performance.
Adopt the prepared matrix material body of the present invention, when emitting, experience a quench process in reactor.This quench process can make the liquid composite material body rapid solidification after melting mixing become solid union material, is conducive to the operation of follow-up pulverising step, enhances productivity; Simultaneously, in quench process, because the water vapor being wrapped in fused solution matrix material can not overflow in time and form vesicular structure in solid union material, thereby improved the loose fragility of matrix material, pitch-the mineral composite making is more easily pulverized, thereby can be made easily the pitch-mineral composite powder material that is applicable to various operating modes.
The present invention also provides pitch-mineral composite of preparing based on above method to be used for the purposes of waterproof roll, bitumen for road use, waste rubber regeneration and petroleum drilling anti-sloughing agent.
The pitch mineral composite that utilizes thick oil sludge to prepare the method for pitch-mineral composite and prepare by the method provided by the invention, has the following advantages:
The first, method provided by the invention, can effectively utilize viscous oil recovery in petroleum industry and containing the thick oil sludge producing in condensed oil sewage treating processes, prepare the product with practical value, realizes the harmless treatment of hazardous and noxious substances, and turns waste into wealth;
The second, compare with traditional treatment method, method provided by the invention, for processing thick oil sludge, to have production technique simple, implement convenient and easy, practical, can large-scale promotion to oil production industry;
The 3rd, the inventive method waste utilization rate is high, realizes recycling and produce on innoxious basis, creates certain economic value when reducing environmental pollution;
The 4th, pitch-mineral composite of preparing according to method provided by the invention approximately contains 2/3rds the oil soluble hydrocarbons such as resin and asphalt, containing 1/3rd ultra tiny inorganic mineral powders, can be widely used in waterproof roll, bitumen for road use, waste rubber regeneration and petroleum drilling anti-sloughing agent etc.;
The 5th, thick oil sludge is prepared into the pitch-mineral composite having compared with high added value, avoided that greasy filth is independent or mixed with coal and be used as the burning of fuel low value, and can produce the toxic and harmful that contains dioxin that causes serious environmental pollution in combustion processes, thick oil sludge is fully used as a kind of precious resources, realizes the clean cycle utilization of " turning waste into wealth " and resource.
Embodiment
High softening point bitumen used in embodiment 1: the rock asphalt that 137 rock asphalt ore deposits of Production and Construction Corps of Xinjiang's agriculture 7 teacher produce, oily molten rate 96%, 160～190 ℃ of softening temperatures (ring and ball method), density (25 ℃) 1.04g/cm
3, 350 ℃ of open flash point >, each main ingredient content is stable hydrocarbon 2%～3%, aromatic hydrocarbon 4～11%, bituminous matter 32%～64%, colloid 30%～54%;
Used oil soluble resin in embodiment 1: No. 10 C9 petroleum resin that Zibo Qi Bang resin processing plant produces, 80～130 ℃ of softening temperatures, oily molten rate 98%;
Gum Rosin used in embodiment 2: the Pro12991816 Gum Rosin that Beichen District, Tianjin Qing Hui afforestation product company limited produces, 100～120 ℃ of softening temperatures;
Brown coal used in embodiment 2: the brown coal powder that Inner Mongol Huo Meizhong section humic acids science and technology limited Company is produced, humic acids content 70%;
Dehydration fusel used in embodiment 3: the dehydration potato spirit that Liu Xiaojie chemical plant, Shenyang produces, main component is the mixture of ethylene glycol, propylene glycol, butyleneglycol, glycerol and oligopolymer thereof;
Used oil soluble resin in embodiment 3: No. 16 C9 petroleum resin that Zibo Qi Bang resin processing plant produces, 80～130 ℃ of softening temperatures, oily molten rate 95%;
The grand resin of groom used in embodiment 4: the coumarone indene resin that Shenzhen Jitian Chemical Co., Ltd. produces, 70～105 ℃ of softening temperatures, oily molten rate 98%;
Plant asphalt used in embodiment 4: the VGA-VA270 plant asphalt that Shanghai DaCheng Co., Ltd produces, 80 ℃ of softening temperatures, kinematic viscosity (60 ℃)>=230 handkerchief second, volatility (163 ℃ * 3h)≤1, density (25 ℃)=1.268g/cm
3, moisture≤1%.
Following embodiment thick oil sludge used is the homogenizing dehydration thick oil sludge sample of Liaohe Oil Field thick oil sludge treatment plant of Hua You group.But, easily understand, for forming the thick oil sludge that similarly other viscous crude fields produce, the technology of the present invention is applicable too.Embodiment 1
(1) take 240kg thick oil sludge, 80kg high softening-point rock asphalt carries out melting after evenly mixing under 200 ℃ of high temperature;
(2) melting stops heating after 60 minutes, add 40kg as No. 10 oil-soluble resins of hard brittle material, utilize the waste heat of high-heat heavy crude greasy filth, make No. 10 oil-soluble resin fusings, be stirred to and in normal temperature clear water, carry out after uniform fluid suddenly coolingly, obtain matrix material body;
(3) the matrix material body making in step (2) is carried out after seasoning in shady and cool ventilation place, it is 100 order powder granules that air blast cooling crush machine is crushed to granularity, obtains embodiment 1 sample.
Embodiment 2
(1) take 240kg thick oil sludge, 100kg Gum Rosin carries out melting under 140 ℃ of high temperature;
(2) melting stops heating after 1 hour, adds 80kg as the brown coal of hard brittle material, utilizes the waste heat of high-heat heavy crude greasy filth, makes brown coal fusings, is stirred in normal temperature clear water, to carry out after uniform fluid suddenly coolingly, obtains matrix material body;
(3) composite material precursors making in step (2) is carried out after seasoning in shady and cool ventilation place, it is 80 order powder granules that air blast cooling crush machine is crushed to granularity, obtains embodiment 2 samples.
Embodiment 3
(1) take 240kg thick oil sludge, 60kg dehydration fusel carries out melting under 120 ℃ of high temperature;
(2) melting stops heating after 40 minutes, add 60kg as No. 16 oil-soluble resins of hard brittle material, utilize the waste heat of high-heat heavy crude greasy filth, make No. 16 oil-soluble resin fusings, be stirred to and in normal temperature clear water, carry out after uniform fluid suddenly coolingly, obtain matrix material body;
(3) the matrix material body making in step (2) is carried out after seasoning in shady and cool ventilation place, it is 60 order powder granules that air blast cooling crush machine is crushed to granularity, obtains embodiment 3 samples.
Embodiment 4
(1) take 240kg thick oil sludge, the grand resin of 60kg groom carries out melting under 100 ℃ of high temperature;
(2) melting stops heating after 1 hour, adds 100kg plant asphalt, utilizes the waste heat of high-heat heavy crude greasy filth, makes plant asphalt fusing, is stirred to be to carry out in normal temperature clear water after uniform fluid suddenly cooling, obtains matrix material body;
(3) composite material precursors making in step (2) carries out after seasoning in shady and cool ventilation place, and it is 100 order powder granules that air blast cooling crush machine is crushed to granularity, obtains embodiment 4 samples.
Experimental example
This experimental example specimen in use is all selected from above-described embodiment 1～4.
Experimental example 1 fineness test
Take sample 50.00g, be placed in 30 mesh standard sieves, shake standard sieve rapidly until sample no longer leaks down, weigh screenings quality, calculate as follows fineness:
In formula: S---fineness (%);
M1---screenings quality (g);
M---take sample mass (g).
The oily molten rate of experimental example 2 detects
(1) get 0.2～0.3g absorbent cotton, a lens wiping paper, one section of line and be placed in weighing bottle, at 105 ℃, dry to constant weight, standby;
(2) the lens wiping paper doubling in (1), be laid on pan paper, then absorbent cotton is evenly laid in to lens wiping paper middle part, take porphyrize and be the sample 0.5g that 0.28mm standard sieve sieved through the sieve aperture length of side, be positioned over absorbent cotton center;
(3) sample in (2) is tight with the degreasing bale of cotton, use again lens wiping paper that cotton winding is tight, finally use the bundle of lines sample looping in (1) good, in ladle sample process, can not there is sample to leak outside, the sample bag of wrapping can not obviously be seen sample, sample bag is put into the sample cup of extractor, sample cup hangs over miniature prolong below in extractor;
(4) in extractor, inject after 250mL tetracol phenixin (76.8 ℃ of boiling points), extractor is put into electric mantle and be heated to 80 ℃ and keep boiling state, till treating that effluent liquid is colourless;
(5) take out sample cup, the paper roll that is surrounded by sample is placed in to loft drier, at 105 ℃, dry 2h, takes out and puts into moisture eliminator, after the cooling 30min of normal temperature, weighs;
(6) calculate as follows oily molten rate:
In formula: W
o---oily molten rate (%);
M
7---sample mass (g);
M
8---absorbent cotton, wiping lens paper and sample mass (g);
M
9---absorbent cotton, wiping lens paper and residue quality (g).
Experimental example 3 softening temperatures detect
By sample, at 280 ℃, after calcination 30min, by GB/T4507-84(, be ring and ball method) carry out softening point measurement.
This experimental example sample used is prepared in embodiment 1～example 4.
Physicochemical property detected result is as shown in table 1 below:
Table 1 embodiment sample physicochemical property quality examination result
It is controlled that pitch-mineral composite of preparing according to method provided by the invention has granularity, the molten rate of oil is higher, softening temperature is lower, process the features such as easy to use, be suitable for waterproof roll, modifying road asphalt, waste Crumb rubber regeneration is softening and the multiple fields such as oil field drilling fluids chemical is used as pitch surrogate, have compared with high performance-price ratio.
Above combination embodiment and exemplary example have been described in detail the present invention, but these explanations can not be interpreted as limitation of the present invention.It will be appreciated by those skilled in the art that in the situation that not departing from spirit and scope of the invention, can carry out multiple replacement of equal value, modify or improve technical solution of the present invention and embodiment thereof, these all fall within the scope of the present invention.Protection scope of the present invention is as the criterion with claims.
Claims (10)
1. pitch-the mineral composite that utilizes thick oil sludge to prepare, is characterized in that, by the composition that comprises following weight proportion, is made:
Thick oil sludge: 40～80 parts;
Softening temperature conditioning agent: 10～30 parts;
Hard brittle material: 5～20 parts,
Wherein,
Described thick oil sludge is the mud containing viscous crude of the outer row of oily water treatment joint station in petroleum industry viscous oil recovery process;
Described hard brittle material is selected from: oil soluble petroleum resin, brown coal or its mixture;
Described softening temperature conditioning agent is selected from: the mixture that one or more arbitrary proportions in Gum Rosin natural or synthetic, dehydration fusel, high softening point bitumen, biological carbon, xylogen and humic acids form, wherein,
Described high softening point bitumen is softening temperature higher than the pitch of 150 ℃;
The multiporous biological carbon of described biological carbon for being processed by organic by-products such as animal excrement, animal bone, plant roots and stems, wood chip or Wheat Straws;
The product that described dehydration fusel obtains after dehydration reaction for be greater than 2 aliphatics alcohols by carbonatoms;
Described pitch-mineral composite is prepared by the following method and is obtained:
(1) by above-mentioned weight proportion, take thick oil sludge and softening temperature conditioning agent evenly mixes, after mixing, under melt temperature is the condition of 80～200 ℃, carry out melting;
(2) in step (1), mixture reaches after molten state, stops heating, adds immediately hard brittle material, utilizes the remaining temperature of mixture that hard brittle material is melted, and is stirred to be in normal-temperature water, to carry out after uniform fluid suddenly coolingly, obtains matrix material body;
(3) the matrix material body through obtaining in step (2) is carried out to seasoning, being ground into particle diameter after to be dried is 60～100 object powder granules.
2. a kind of pitch-mineral composite that utilizes thick oil sludge to prepare according to claim 1, is characterized in that, comprises the composition of following weight proportion:
Thick oil sludge: 55～75 parts;
Softening temperature conditioning agent: 15～22 parts;
Hard brittle material: 10～15 parts;
Described in step (1), melt temperature is 100～150 ℃;
Described in step (3), crushing process carries out in air blast cooling crush machine;
Described high softening point bitumen is softening temperature higher than the pitch of 180 ℃.
3. a kind of pitch-mineral composite that utilizes thick oil sludge to prepare according to claim 1, it is characterized in that, described high softening point bitumen is the pitch of 190～260 ℃ of softening temperatures, is selected from: originate from the mixture that one or more arbitrary proportions in the rock asphalt on the ground such as Xinjiang, Sichuan, Iran form.
4. utilize thick oil sludge to prepare a method for pitch-mineral composite, it is characterized in that, comprise the following steps:
(1) take thick oil sludge and softening temperature conditioning agent evenly mixes, after mixing, under melt temperature is the condition of 80～200 ℃, carry out melting;
(2) in step (1), mixture reaches after molten state, stops heating, adds immediately hard brittle material, utilizes the remaining temperature of mixture that hard brittle material is melted, and is stirred to be in normal-temperature water, to carry out after uniform fluid suddenly coolingly, obtains matrix material body;
(3) the matrix material body through obtaining in step (2) is carried out to seasoning, being ground into particle diameter after to be dried is 60～100 object powder granules,
Wherein,
Described thick oil sludge is the mud containing viscous crude of the outer row of oily water treatment joint station in petroleum industry viscous oil recovery process;
Described hard brittle material is selected from: oil soluble petroleum resin, brown coal or its mixture;
Described softening temperature conditioning agent is selected from: the mixture that one or more arbitrary proportions in Gum Rosin natural or synthetic, dehydration fusel, high softening point bitumen, biological carbon, xylogen and humic acids form, wherein,
Described high softening point bitumen is softening temperature higher than the pitch of 150 ℃;
The multiporous biological carbon of described biological carbon for being processed by organic by-products such as animal excrement, animal bone, plant roots and stems, wood chip or Wheat Straws;
Described dehydration fusel is, by carbonatoms, is greater than the product that 2 aliphatics alcohols obtains after dehydration reaction.
5. a kind of method of utilizing thick oil sludge to prepare pitch-mineral composite according to claim 4, is characterized in that,
Described in step (1), melt temperature is 100～150 ℃;
Described in step (3), crushing process carries out in air blast cooling crush machine;
Described high softening point bitumen is softening temperature higher than the pitch of 180 ℃.
6. a kind of method of utilizing thick oil sludge to prepare pitch-mineral composite according to claim 4, it is characterized in that, described high softening point bitumen is the pitch of 190～260 ℃ of softening temperatures, is selected from: originate from the mixture that one or more arbitrary proportions in the rock asphalt on the ground such as Xinjiang, Sichuan, Iran form.
7. a kind of method of utilizing thick oil sludge to prepare pitch-mineral composite according to claim 4, is characterized in that, comprises the composition of following weight proportion:
Thick oil sludge: 40～80 parts;
Softening temperature conditioning agent: 10～30 parts;
Hard brittle material: 5～20 parts.
8. a kind of method of utilizing thick oil sludge to prepare pitch-mineral composite according to claim 4, is characterized in that, comprises the composition of following weight proportion:
Thick oil sludge: 55～75 parts;
Softening temperature conditioning agent: 15～22 parts;
Hard brittle material: 10～15 parts.
9. one kind is utilized pitch-mineral composite prepared by thick oil sludge to be used for the purposes that waterproof roll, bitumen for road use and waste rubber are regenerated.
10. one kind is utilized pitch-mineral composite prepared by thick oil sludge for the purposes of petroleum drilling anti-sloughing agent.
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| CN106147252A (en) * | 2014-11-03 | 2016-11-23 | 中国石油化工股份有限公司 | A kind of preparation method of environment-friendly type asphalt mixture additive |
| CN106147248A (en) * | 2014-11-03 | 2016-11-23 | 中国石油化工股份有限公司 | A kind of asphalt mixture warm-mixing additive and preparation method thereof |
| CN106147252B (en) * | 2014-11-03 | 2018-07-20 | 中国石油化工股份有限公司 | A kind of preparation method of environment-friendly type asphalt mixture additive |
| CN106147248B (en) * | 2014-11-03 | 2018-12-21 | 中国石油化工股份有限公司 | A kind of asphalt mixture warm-mixing additive and preparation method thereof |
| CN106147250A (en) * | 2015-04-13 | 2016-11-23 | 中国石油化工股份有限公司 | A kind of warm-mixed asphalt and preparation method thereof |
| CN106147249A (en) * | 2015-04-13 | 2016-11-23 | 中国石油化工股份有限公司 | A kind of warm mix type Rut resistance composite modifier and preparation method thereof |
| CN106147251A (en) * | 2015-04-13 | 2016-11-23 | 中国石油化工股份有限公司 | A kind of warm-mixed asphalt additive and preparation method thereof |
| CN106147250B (en) * | 2015-04-13 | 2019-01-25 | 中国石油化工股份有限公司 | A kind of warm-mixed asphalt and preparation method thereof |
| CN106147251B (en) * | 2015-04-13 | 2019-01-25 | 中国石油化工股份有限公司 | A kind of warm-mixed asphalt additive and preparation method thereof |
| CN106147249B (en) * | 2015-04-13 | 2019-07-12 | 中国石油化工股份有限公司 | A kind of warm mix type Rut resistance composite modifier and preparation method thereof |
| CN105017788A (en) * | 2015-07-16 | 2015-11-04 | 长安大学 | Methods for modifying asphalt and mixture thereof by using biochar |
| CN106045383A (en) * | 2016-05-27 | 2016-10-26 | 长安大学 | Agricultural waste residue ash and modified asphalt mixture and method for preparing same |
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