CN103554936B - A kind of pitch-mineral composite utilizing thick oil sludge to prepare and preparation method thereof - Google Patents

A kind of pitch-mineral composite utilizing thick oil sludge to prepare and preparation method thereof Download PDF

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CN103554936B
CN103554936B CN201310567507.0A CN201310567507A CN103554936B CN 103554936 B CN103554936 B CN 103554936B CN 201310567507 A CN201310567507 A CN 201310567507A CN 103554936 B CN103554936 B CN 103554936B
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pitch
thick oil
oil sludge
prepare
mineral composite
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CN201310567507.0A
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CN103554936A (en
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周风山
张以河
宋启辉
仝坤
刘建中
王焕娜
孟祥海
曹灿
李德华
张皓
王恩旭
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辽河石油勘探局
中国地质大学(北京)
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Abstract

The invention provides one utilizes thick oil sludge to prepare the method for pitch-mineral composite, comprise: after thick oil sludge mixes with softening temperature conditioning agent, carry out high-temperature fusion, after stopping heating, add hard brittle material, the remaining temperature of the former two's mixture is utilized to be melted, suddenly cool after being stirred to uniform fluid, the step such as drying, pulverizing makes pitch-mineral composite again, method provided by the invention realizes its recycling on the innoxious basis of thick oil sludge, can create certain economic value while reducing environmental pollution; The invention also discloses a kind of pitch-mineral composite adopting the method to prepare, products obtained therefrom can be applicable to the multiple fields such as waterproof roll, road bitumen, waste Crumb rubber regeneration and oil field chemical, non-secondary pollution.

Description

A kind of pitch-mineral composite utilizing thick oil sludge to prepare and preparation method thereof

Technical field

The present invention relates to the recycling field of thick oil sludge, particularly viscous oil recovery and the innoxious and recycling containing the thick oil sludge produced in condensed oil sewage treating processes in a kind of petroleum industry.

Background technology

Thick oil sludge is mainly derived from the oily sludge produced in viscous crude field Oil extraction process and in oil field gathering and transportation process, mainly comprises the residual active sludge after the oil trap bed mud of sewage treatment system of oilfield generation, tank bed mud, scum bottom sludge and biochemical wastewater treatment.In thick oil sludge, resin and asphalt component concentration is high, clay mineral content in colloidal form in conjunction with existence is also higher, this two classes material is the main nonaqueous component of thick oil sludge, its viscosity is large, density is large, not easily dewaters, 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 containing a large amount of aged 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.Add the water treatment agent such as a large amount of degreaser, organic and inorganic flocculating agent, inhibiter, Scale inhibitors, sterilant in simultaneously viscous oil recovery and condensed oil sewage treating processes, wherein solid phase is based on clay minerals impurity; Liquid phase part is mainly the sufficient emulsion of emulsification, and form is oil-in-water (O/W) or water-in-oil (W/O).Due to composition and the character complexity of thick oil sludge, intractability is large, there is again the features such as low nutrition thing, low-permeability, nutrition and oxygen skewness simultaneously, therefore its poor stability, easy corruption and generation stench, particularly to have the material of foul smell and toxicity very harmful for benzene homologues, phenol, pyrene etc. wherein, belongs to HW08 class organic hazardous waste of regulation in China " National Hazard refuse register " (version in 2008), and serious threat is to the life of the people and health.

Tradition disposal of oily sludge pattern mainly comprises following several: 1. solidify, and adopts the materials such as cement by landfill after thick oil sludge solidification, reduces the harm to environment; 2. centrifugal, for the greasy filth that solids content is high, although after this process in greasy filth oleaginousness still very high, can recovery part crude oil; 3. dewater, burn, the method solves greasy filth comparatively up hill and dale and pollutes, but it is high to there is equipment power consumption, the phenomenons such as crude resources waste, and is difficult to the long-time running of guarantee equipment.

The technology related to during recent domestic process oily sludge mainly comprises sludge pretreatment, thermal treatment, solvent extraction process, biological treatment and comprehensive utilization etc.Such as US Patent No. Pat.6673231 uses pyrogen oil flushing tank bed mud, then carries out distillation process, and its treatment effect is good, but cost intensive, and energy consumption is large.A kind of process for treating oil-containing sludge of Chinese patent CN200710145460 disclosure of the invention, comprise concentration, the step such as flocculation-centrifuge dehydration and drying and other treatment, its technological process is loaded down with trivial details, though length consuming time, the environmental benefit of achieving, does not have economic benefit.Chinese patent CN201110080196 discloses oily sludge and focuses on the treatment process with recycling, the method obtains mud cake and sewage through multistep dehydration separation, utilize as moulded coal mixed material, but the method cyclic step is too much, installation cost is too high.World patent WO2011074007 and US Patent No. Pat.2008264856 carries out bioreediation to oily sludge respectively, and utilize microorganism to carry out oil removal treatment, but cost is higher, process is wayward.World patent WO2009028518, Chinese patent CN201338974 and US Patent No. Pat.20060012970 distinguish the research and design treatment unit of several different oily sludge, this class methods initial outlay is larger, ageing not strong, treatment effect is unstable, different because of oil.

Chinese patent CN101045600A provides a kind for the treatment of process of thick oil sludge bituminous grouting, technical scheme comprises: the thick oil sludge that (1) gets oil removal after pretreatment, flotation produces, be positioned in batch type reactor, heat up under mechanical stirring 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 DEG C, 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: the moisture 1. in thick oil sludge, oil content and solid have formed stable emulsified state, not easily distill under low temperature, in the course of processing, temperature needs up to 370 DEG C, therefore, the high energy consumption that pyroreaction causes can cause cost to remain 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 yields is little, quality is low, its economy is unsatisfactory.

Summary of the invention

For solving the problems of the technologies described above, the present inventor is through studying 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 utilizing thick oil sludge to prepare, it is characterized in that, be made up of the composition comprising following weight proportion:

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 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: natural or the Gum Rosin of synthetic, the mixture of one or more arbitrary proportions formation of dewatering in fusel, high softening point bitumen, biological carbon, xylogen and humic acids, wherein,

Described high softening point bitumen is softening temperature higher than the pitch of 150 DEG C;

Described biological carbon is the multiporous biological carbon processed by organic by-products such as animal excrement, animal bone, plant roots and stems, wood chip or Wheat Straws;

Described dehydration fusel is the product that the aliphatics alcohols being greater than 2 by carbonatoms obtains after dehydration reaction;

Described pitch-mineral composite is prepared by following steps and obtains:

(1) taking thick oil sludge and softening temperature conditioning agent Homogeneous phase mixing by above-mentioned weight proportion, is carry out melting under the condition of 80 ~ 200 DEG C in melt temperature after mixing;

(2), after mixture reaches molten state in step (1), stop heating, add hard brittle material immediately, utilize the remaining temperature of mixture to be melted by hard brittle material, be stirred to and suddenly cool in normal-temperature water in after uniform fluid, obtain composite body;

(3) composite body obtained in step (2) is carried out 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 utilizing thick oil sludge to prepare, it is characterized in that, comprise 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 DEG C;

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 DEG C.

The third aspect, the invention provides above-mentioned a kind of pitch-mineral composite utilizing thick oil sludge to prepare, it is characterized in that, described high softening point bitumen is the pitch of softening temperature 190 ~ 260 DEG C, 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 are formed.

Fourth aspect, the invention provides one and utilizes thick oil sludge to prepare the method for pitch-mineral composite, it is characterized in that, comprise the following steps:

(1) taking thick oil sludge and softening temperature conditioning agent Homogeneous phase mixing, is carry out melting under the condition of 80 ~ 200 DEG C in melt temperature after mixing;

(2), after mixture reaches molten state in step (1), stop heating, add hard brittle material immediately, utilize the remaining temperature of mixture to be melted by hard brittle material, be stirred to and suddenly cool in normal-temperature water in after uniform fluid, obtain composite body;

(3) composite body obtained in step (2) is carried out seasoning, being ground into particle diameter after to be dried is 60 ~ 100 object powder granules,

Wherein,

Described thick oil sludge be in petroleum industry viscous oil recovery process oily water treatment joint station arrange outward containing heavy crude oily sludge;

Described hard brittle material is selected from: oil soluble petroleum resin, brown coal or its mixture;

Described softening temperature conditioning agent is selected from: natural or the Gum Rosin of synthetic, the mixture of one or more arbitrary proportions formation of dewatering in fusel, high softening point bitumen, biological carbon, xylogen and humic acids, wherein,

Described high softening point bitumen is softening temperature higher than the pitch of 150 DEG C;

Described biological carbon is the multiporous biological carbon processed by organic by-products such as animal excrement, animal bone, plant roots and stems, wood chip or Wheat Straws;

Described dehydration fusel is, the product that the aliphatics alcohols being greater than two by carbonatoms obtains after dehydration reaction.

5th aspect, the invention provides above-mentioned one and utilizes thick oil sludge to prepare the method for pitch-mineral composite, it is characterized in that,

Described in step (1), melt temperature is 100 ~ 150 DEG C;

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 DEG C.

6th aspect, the invention provides above-mentioned one utilizes thick oil sludge to prepare the method for pitch-mineral composite, it is characterized in that, described high softening point bitumen is the pitch of softening temperature 190 ~ 260 DEG C, 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 are formed.

7th aspect, the invention provides above-mentioned one and utilizes thick oil sludge to prepare the method for pitch-mineral composite, it is characterized in that, comprise 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.

Eighth aspect, the invention provides above-mentioned one and utilizes thick oil sludge to prepare the method for pitch-mineral composite, it is characterized in that, comprise 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.

9th aspect, the invention provides the purposes that a kind of pitch-mineral composite utilizing thick oil sludge to prepare is used for the regeneration of waterproof roll, bitumen for road use and waste rubber.

Tenth aspect, the invention provides the purposes that a kind of pitch-mineral composite utilizing thick oil sludge to prepare is used for petroleum drilling anti-sloughing agent.

According to provided by the invention a kind of utilize thick oil sludge to prepare pitch-mineral composite method and by pitch mineral composite prepared by the method, there is following beneficial effect:

(1) method provided by the invention, effectively can utilize viscous oil recovery in petroleum industry and containing the thick oil sludge produced in condensed oil sewage treating processes, prepare the product with practical value, realize the harmless treatment of hazardous and noxious substances, and turn waste into wealth;

(2) compared with traditional treatment method, method provided by the invention, has production technique for process thick oil sludge simple, implements convenient and easy, practical, can large-scale promotion in oil production industry;

(3) the inventive method waste utilization rate is high, innoxious basis realizes recycling and produces, create certain economic value while reducing environmental pollution;

(4) pitch-mineral composite prepared according to method provided by the invention about contains the oil soluble hydrocarbons such as the resin and asphalt of 2/3rds, containing 1/3rd ultra tiny inorganic mineral powders, waterproof roll, bitumen for road use, waste rubber regeneration and petroleum drilling anti-sloughing agent etc. can be widely used in;

(5) thick oil sludge is prepared into the pitch-mineral composite had compared with high added value, avoid by greasy filth separately or mix with coal and be used as fuel low value and burn, and avoid the toxic and harmful containing dioxin that the meeting produced in combustion causes Heavy environmental pollution.

Embodiment

Further explain and describe content of the present invention by the following examples.But the embodiment provided should not be understood to be construed as limiting scope.

The invention provides a kind of pitch-mineral composite utilizing 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 of following weight proportion is comprised:

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 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, such as, and 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.Add hard brittle material preparing in pitch-mineral composite process, prepared pitch-mineral composite can be made 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: natural or the Gum Rosin of synthetic, the mixture of one or more arbitrary proportions formation of dewatering in fusel, high softening point bitumen, biological carbon, xylogen and humic acids.

Pitch-mineral composite that the thick oil sludge with high softening-point is prepared can present the solid composite material characteristic of class sapropelitic at normal temperatures, pitch-mineral composite that the thick oil sludge of low softening point is prepared is then without this characteristic, but, the present invention is used as to there is the lower resin and asphalt component of a large amount of softening temperatures in the thick oil sludge of raw material, therefore need to add high softening-point material to heighten the softening temperature of thick oil sludge, thus prepare required pitch-mineral composite, in addition, because the softening temperature of thick oil sludge is lower, easily there is the unfavorable side reactions such as carburizing reagent in high-temperature fusion process, for avoiding the generation of this type of side reaction, softening temperature conditioning agent is added in melting process, thus 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 DEG C, and preferably higher than 180 DEG C, preferred softening temperature is 190 ~ 260 DEG C.

Biological carbon be a kind of organic carbon of fragility, the softening temperature that biological carbon had both been conducive to the pitch-mineral composite prepared by raising is added in thick oil sludge, also be conducive to the fragility of the pitch-mineral composite prepared by increase, thus be convenient to the pulverizing of follow-up pitch-mineral composite.The preferred biological carbon of the present invention is the multiporous biological carbon 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 mixed by bio-alcohol industrial by-products, and its main component is dibasic alcohol, trivalent alcohol and low-molecular(weight)polymer thereof.Under the high temperature conditions, esterification occurs for carboxyl, amido etc. contained by abundant hydroxyl contained in fusel and colloid, bituminous matter and (or) cross-linking chemistry reacts, generate the netted condensed ring macromole with more high molecular, this condensed ring macromole can strengthen colloid, bitum cementability and toughness, the visco-elasticity of the matrix material prepared by improvement, makes it really have the viscous-elastic behaviour of class sapropelitic.The dehydration fusel that the present invention selects is the product that the aliphatics alcohols being greater than 2 by carbonatoms obtains after dehydration reaction, such as primarily of the mixture of ethylene glycol, propylene glycol, butyleneglycol, glycerol and oligopolymer thereof composition, but be not limited to cited dehydration fusel example.

The invention provides a kind of method utilizing thick oil sludge to prepare pitch-mineral composite, particularly, comprise the following steps:

(1) taking thick oil sludge and softening temperature conditioning agent Homogeneous phase mixing, is carry out melting under the condition of 80 ~ 200 DEG C in melt temperature after mixing;

(2), after mixture reaches molten state in step (1), stop heating, add hard brittle material immediately, utilize the remaining temperature of mixture to be melted by hard brittle material, be stirred to and suddenly cool in normal-temperature water in after uniform fluid, obtain composite body;

(3) composite body obtained in step (2) is carried out 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 is solid-state or semi-solid state under normal temperature, wherein containing a large amount of resin and asphalt material, 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 more than its fusing point, namely more than 80 DEG C time, can melting mutual to 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 comparatively thick oil sludge and softening temperature conditioning agent low, therefore can plant after component melts mixes at the first two and add hard brittle material, the melting of hard brittle material can be realized by means of its waste heat, thus save energy cost, but melt temperature is unsuitable too high, and when temperature is higher than 200 DEG C, thick oil sludge carburizing reagent can occur, thus causes the reduction of composite products performance.

Adopting the composite body prepared by the present invention, experiencing a quench process when releasing in reactor.Liquid composite material body rapid solidification after this quench process can make melting mixing becomes solid union material, is conducive to the operation of follow-up pulverising step, enhances productivity; Simultaneously, in quench process, in solid union material, vesicular structure is formed because the water vapor be wrapped in fused solution matrix material can not overflow in time, thus improve the loose fragility of matrix material, pitch-the mineral composite obtained more easily is pulverized, thus the pitch-mineral composite powder material being applicable to various operating mode can be obtained easily.

Present invention also offers the purposes that pitch-mineral composite of preparing based on above method is used for waterproof roll, bitumen for road use, waste rubber regeneration and petroleum drilling anti-sloughing agent.

Provided by the invention utilize thick oil sludge to prepare pitch-mineral composite method and by pitch mineral composite prepared by the method, have the following advantages:

The first, method provided by the invention, effectively can utilize viscous oil recovery in petroleum industry and containing the thick oil sludge produced in condensed oil sewage treating processes, prepare the product with practical value, realize the harmless treatment of hazardous and noxious substances, and turn waste into wealth;

The second, compared with traditional treatment method, method provided by the invention, has production technique for process thick oil sludge simple, implements convenient and easy, practical, can large-scale promotion in oil production industry;

3rd, the inventive method waste utilization rate is high, innoxious basis realizes recycling and produces, create certain economic value while reducing environmental pollution;

4th, the oil soluble hydrocarbons such as the resin and asphalt of 2/3rds are about contained according to pitch-mineral composite prepared by method provided by the invention, containing 1/3rd ultra tiny inorganic mineral powders, waterproof roll, bitumen for road use, waste rubber regeneration and petroleum drilling anti-sloughing agent etc. can be widely used in;

5th, thick oil sludge is prepared into the pitch-mineral composite had compared with high added value, avoid by greasy filth separately or mix with coal and be used as fuel low value and burn, and the toxic and harmful containing dioxin causing Heavy environmental pollution can be produced in combustion, thick oil sludge is fully used as a kind of precious resources, realizes " turning waste into wealth " and utilize with the clean cycle of resource.

Embodiment

High softening point bitumen used in embodiment 1: the rock asphalt that Production and Construction Corps of Xinjiang's agriculture 7 teacher 137 rock asphalt ore deposits produce, oil solution ratio 96%, softening temperature (ring and ball method) 160 ~ 190 DEG C, density (25 DEG C) 1.04g/cm 3, open flash point > 350 DEG C, 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, softening temperature 80 ~ 130 DEG C, oil solution ratio 98%;

Gum Rosin used in embodiment 2: the Pro12991816 Gum Rosin that Beichen District, Tianjin Qing Hui afforestation product company limited produces, softening temperature 100 ~ 120 DEG C;

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, softening temperature 80 ~ 130 DEG C, oil solution ratio 95%;

The grand resin of groom used in embodiment 4: the coumarone indene resin that Jitian Chemical Co., Ltd. of Shenzhen produces, softening temperature 70 ~ 105 DEG C, oil solution ratio 98%;

Plant asphalt used in embodiment 4: the VGA-VA270 plant asphalt that Shanghai DaCheng Co., Ltd produces, softening temperature 80 DEG C, kinematic viscosity (60 DEG C)>=230 handkerchief second, volatility (163 DEG C × 3h)≤1, density (25 DEG C)=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 easy understand, for the thick oil sludge that other viscous crude fields that composition is similar produce, the technology of the present invention is suitable for too.Embodiment 1

(1) take 240kg thick oil sludge, after 80kg high softening-point rock asphalt Homogeneous phase mixing, under 200 DEG C of high temperature, carry out melting;

(2) melting stops heating after 60 minutes, add No. 10 oil-soluble resins of 40kg as hard brittle material, utilize the waste heat of high-heat heavy crude greasy filth, make No. 10 oil-soluble resin fusings, suddenly cool in normal temperature clear water after being stirred to uniform fluid, obtain composite body;

(3), after composite body obtained in step (2) being carried out 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 DEG C of high temperature;

(2) melting stops heating after 1 hour, adds the brown coal of 80kg as hard brittle material, utilizes the waste heat of high-heat heavy crude greasy filth, brown coal are melted, suddenly cool, obtain composite body after being stirred to uniform fluid in normal temperature clear water;

(3), after composite material precursors obtained in step (2) being carried out 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 sample.

Embodiment 3

(1) take 240kg thick oil sludge, 60kg dehydration fusel carries out melting under 120 DEG C of high temperature;

(2) melting stops heating after 40 minutes, add No. 16 oil-soluble resins of 60kg as hard brittle material, utilize the waste heat of high-heat heavy crude greasy filth, make No. 16 oil-soluble resin fusings, suddenly cool in normal temperature clear water after being stirred to uniform fluid, obtain composite body;

(3), after composite body obtained in step (2) being carried out 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 sample.

Embodiment 4

(1) take 240kg thick oil sludge, the grand resin of 60kg groom carries out melting under 100 DEG C 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, plant asphalt is melted, be suddenly to cool in normal temperature clear water, obtain composite body after being stirred to uniform fluid;

(3), after obtained in step (2) composite material precursors carries out 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 4 sample.

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, vibrations standard sieve is till sample no longer leaks down rapidly, weighs screenings quality, calculates fineness as follows:

S = m 1 m × 100 %

In formula: S---fineness (%);

M1---screenings quality (g);

M---take sample mass (g).

Experimental example 2 oil solution ratio detects

(1) get 0.2 ~ 0.3g absorbent cotton, lens wiping paper, one section of line are placed in weighing bottle, dry at 105 DEG C to constant weight, for subsequent use;

(2) the lens wiping paper doubling in (1), be laid on pan paper, then absorbent cotton is evenly laid in the middle part of lens wiping paper, take porphyrize and be the sieved sample 0.5g of 0.28mm standard sieve through the sieve aperture length of side, be positioned over absorbent cotton center;

(3) by tight for the sample degreasing bale of cotton in (2), use lens wiping paper tight for cotton winding again, finally use the bundle of lines sample looping in (1) good, sample can not be had in ladle sample process to leak outside, the sample bag wrapped obviously can not see sample, sample bag is put into the sample cup of extractor, sample cup to hang in extractor below miniature prolong;

(4), inject 250mL tetracol phenixin (boiling point 76.8 DEG C) in extractor after, extractor is put into electric mantle and be heated to 80 DEG C and keep boiling state, till treating that effluent liquid is colourless;

(5) take out sample cup, the paper roll being surrounded by sample is placed in loft drier, dry 2h at 105 DEG C, take out and put into moisture eliminator, weigh after normal temperature cooling 30min;

(6) oil solution ratio is calculated as follows:

W o = m 8 - m 9 m 7 × 100

In formula: W o---oil solution ratio (%);

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 temperature detects

By sample at 280 DEG C after calcination 30min by GB/T4507-84(and ring and ball method) carry out softening point measurement.

This experimental example sample used is for prepared by embodiment 1 ~ example 4.

Physicochemical property detected result is as shown in table 1 below:

Table 1 embodiment sample physicochemical property quality measurements

According to method provided by the invention prepare that pitch-mineral composite has granularity is controlled, oil solution ratio is higher, softening temperature is lower, process the features such as easy to use, be suitable for the multiple fields such as the softening and oil field drilling fluids chemical of waterproof roll, modifying road asphalt, waste Crumb rubber regeneration to use as pitch surrogate, there is comparatively high performance-price ratio.

More than in conjunction with embodiment and exemplary example to invention has been detailed description, but these explanations can not be interpreted as limitation of the present invention.It will be appreciated by those skilled in the art that when not departing from spirit and scope of the invention, can carry out multiple equivalencing, modification or improvement to 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 (14)

1. utilize pitch-mineral composite prepared by thick oil sludge, it is characterized in that, be made up of the composition comprising following weight proportion:
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 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: natural or the Gum Rosin of synthetic, the mixture of one or more arbitrary proportions formation of dewatering in fusel, high softening point bitumen, biological carbon, xylogen and humic acids, wherein,
Described high softening point bitumen is softening temperature higher than the pitch of 150 DEG C;
Described biological carbon is the multiporous biological carbon processed by organic by-products;
Described dehydration fusel is the product that the aliphatics alcohols being greater than 2 by carbonatoms obtains after dehydration reaction;
Described pitch-mineral composite is prepared by the following method and obtains:
(1) taking thick oil sludge and softening temperature conditioning agent Homogeneous phase mixing by above-mentioned weight proportion, is carry out melting under the condition of 80 ~ 200 DEG C in melt temperature after mixing;
(2) after in step (1), mixture reaches molten state, stop heating, add hard brittle material immediately, utilize the remaining temperature of mixture to be melted by hard brittle material, be stirred to and suddenly cool in normal-temperature water in after uniform fluid, obtain composite body;
(3) composite body obtained in step (2) is carried out seasoning, being ground into particle diameter after to be dried is 60 ~ 100 object powder granules.
2. a kind of pitch-mineral composite utilizing thick oil sludge to prepare according to claim 1, it is characterized in that, described organic by-products is selected from animal excrement, animal bone, plant roots and stems, wood chip or Wheat Straw.
3. a kind of pitch-mineral composite utilizing thick oil sludge to prepare according to claim 1 and 2, is characterized in that, comprise 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 DEG C;
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 DEG C.
4. a kind of pitch-mineral composite utilizing thick oil sludge to prepare according to claim 1 and 2, is characterized in that, described high softening point bitumen is the pitch of softening temperature 190 ~ 260 DEG C.
5. a kind of pitch-mineral composite utilizing thick oil sludge to prepare according to claim 4, it is characterized in that, described high softening point bitumen is selected from: originate from the mixture that one or more arbitrary proportions in the rock asphalt of Xinjiang, Sichuan, Iran are formed.
6. utilize thick oil sludge to prepare a method for pitch-mineral composite, it is characterized in that, comprise the following steps:
(1) taking thick oil sludge and softening temperature conditioning agent Homogeneous phase mixing, is carry out melting under the condition of 80 ~ 200 DEG C in melt temperature after mixing;
(2) after in step (1), mixture reaches molten state, stop heating, add hard brittle material immediately, utilize the remaining temperature of mixture to be melted by hard brittle material, be stirred to and suddenly cool in normal-temperature water in after uniform fluid, obtain composite body;
(3) composite body obtained in step (2) is carried out 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 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: natural or the Gum Rosin of synthetic, the mixture of one or more arbitrary proportions formation of dewatering in fusel, high softening point bitumen, biological carbon, xylogen and humic acids, wherein,
Described high softening point bitumen is softening temperature higher than the pitch of 150 DEG C;
Described biological carbon is the multiporous biological carbon processed by organic by-products;
Described dehydration fusel is, the product that the aliphatics alcohols being greater than 2 by carbonatoms obtains after dehydration reaction.
7. one utilizes thick oil sludge to prepare the method for pitch-mineral composite according to claim 6, it is characterized in that, described organic by-products is selected from animal excrement, animal bone, plant roots and stems, wood chip or Wheat Straw.
8. according to claim 6 or 7, one utilizes thick oil sludge to prepare the method for pitch-mineral composite, it is characterized in that,
Described in step (1), melt temperature is 100 ~ 150 DEG C;
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 DEG C.
9. according to claim 6 or 7, one utilizes thick oil sludge to prepare the method for pitch-mineral composite, it is characterized in that, described high softening point bitumen is the pitch of softening temperature 190 ~ 260 DEG C.
10. one utilizes thick oil sludge to prepare the method for pitch-mineral composite according to claim 9, it is characterized in that, described high softening point bitumen is selected from: originate from the mixture that one or more arbitrary proportions in the rock asphalt of Xinjiang, Sichuan, Iran are formed.
11. according to claim 6 or 7 one utilize thick oil sludge to prepare the method for pitch-mineral composite, it is characterized in that, comprise 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.
12. according to claim 6 or 7 one utilize thick oil sludge to prepare the method for pitch-mineral composite, it is characterized in that, comprise 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.
13. are used for the purposes of waterproof roll, bitumen for road use and waste rubber regeneration according to a kind of pitch-mineral composite utilizing thick oil sludge to prepare one of Claims 1 to 5 Suo Shu.
14. are used for the purposes of petroleum drilling anti-sloughing agent according to a kind of pitch-mineral composite utilizing thick oil sludge to prepare one of Claims 1 to 5 Suo Shu.
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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
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