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 PDFInfo
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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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- Treatment Of Sludge (AREA)
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
Technical Field
The invention relates to the field of resource utilization of thick oil sludge, in particular to harmless and resource utilization of thick oil sludge generated in the processes of thick oil exploitation and thick oil-containing sewage treatment in the petroleum industry.
Background
The heavy oil sludge is mainly derived from oily sludge generated in the crude oil exploitation process of a heavy oil field and the oil field gathering and transportation process, and mainly comprises bottom sludge of an oil separation tank, bottom sludge of a tank, scum bottom sludge and residual activated sludge generated after biochemical treatment of sewage generated by an oil field sewage treatment system. The thick oil sludge has high content of colloid and asphaltene components, the clay mineral content in the combination of the colloid is higher, the two substances are the most main non-aqueous components of the thick oil sludge, the viscosity and the density are high, the thick oil sludge is not easy to dehydrate, and common oil-containing sludge treatment methods such as drying reduction, solvent extraction, stripping, leaching, solvent extraction-ultrasonic separation, incineration, oxidation, bioremediation, microbial demulsification and the like are not suitable for treating the thick oil sludge.
The heavy oil sludge has complex components, belongs to a multiphase system, and contains a large amount of aged crude oil, wax, asphaltene, colloid, solid suspended matters, bacteria, salts, acid gas, corrosion products, a small amount of heavy metals, oxidants, salts and the like. Meanwhile, a large amount of water treatment agents such as oil removal agents, organic and inorganic flocculants, corrosion inhibitors, scale inhibitors, bactericides and the like are added in the processes of thickened oil exploitation and thickened oil sewage treatment, wherein the solid phase mainly contains clay mineral impurities; the liquid phase part is mainly emulsion with sufficient emulsification, and is in the form of oil-in-water (O/W) or water-in-oil (W/O). The heavy oil sludge has the characteristics of complex composition and properties, high treatment difficulty, low nutrient content, low permeability, uneven distribution of nutrient and oxygen and the like, so the heavy oil sludge has poor stability, is easy to decay and generate malodor, particularly, substances such as benzene series, phenol, pyrene and the like with malodor and toxicity have great harm, belong to HW08 organic hazardous wastes specified in national hazardous waste records (2008 edition), and seriously threaten the life and health of people.
The traditional oily sludge treatment modes mainly comprise the following modes: firstly, solidification, namely, the thick oil sludge is solidified and then buried by adopting materials such as cement and the like, so that the harm to the environment is reduced; centrifuging, namely, aiming at the oil sludge with high solid content, although the oil content in the treated oil sludge is still high, part of crude oil can be recovered; the method can thoroughly solve the oil sludge pollution, but has the phenomena of high equipment energy consumption, crude oil resource waste and the like, and is difficult to ensure the long-term operation of the equipment.
In recent years, technologies related to treatment of oily sludge at home and abroad mainly comprise sludge pretreatment, heat treatment, solvent extraction treatment, biological treatment, comprehensive utilization and the like. For example, U.S. Pat. No. 6673231 uses hot crude oil to wash tank bottom mud, and then carries out distillation treatment, which has good treatment effect, but high cost and large energy consumption. The invention of Chinese patent CN200710145460 discloses an oil-containing sludge treatment method, which comprises the steps of concentration treatment, flocculation-centrifugal dehydration, drying treatment and the like, and has the advantages of complex process and long time consumption, and although the environmental benefit is realized, the economic benefit is not realized. Chinese patent CN201110080196 discloses a centralized treatment and resource utilization method for oil-containing sludge, which obtains sludge cakes and sewage through multi-step dehydration and separation, and uses the sludge cakes and sewage as a mixture of molded coal, but the method has too many reciprocating circulation steps and too high device cost. World patent WO2011074007 and US patent USPat.2008264856 carry out biological decontamination to oily sludge respectively, utilize microorganism to carry out deoiling treatment, but the cost is higher, and the process is difficult to control. World patent WO2009028518, Chinese patent CN201338974 and U.S. Pat. No. 20060012970 respectively study and design several different treatment devices for oil-containing sludge, and the method has the advantages of large initial investment, low timeliness, unstable treatment effect and difference of oil.
Chinese patent CN101045600A provides a treatment method for thick oil sludge asphaltization, and the technical scheme includes: (1) placing the thick oil sludge generated by oil separation and flotation after pretreatment in an intermittent stirring reaction kettle, heating by raising the temperature under mechanical stirring, simultaneously starting a vacuum pump, distilling under reduced pressure, leading out water vapor and oil gas, and then condensing and recovering; (2) and when the temperature reaches 330-370 ℃, keeping the temperature until the oil gas is not distilled out of the kettle, stopping heating, taking out the residual substances in the kettle, and cooling and forming to obtain the asphaltized product. However, the above process has the following defects: firstly, water, oil and solids in the thick oil sludge form a stable emulsified state, the thick oil sludge is not easy to distill at low temperature, and the temperature in the processing process needs to be as high as 370 ℃, so that the cost is high due to high energy consumption caused by high-temperature reaction, and meanwhile, the adhesive force serving as the most main performance of asphalt is greatly reduced due to high-temperature processing, so that the quality of the asphalt is seriously damaged; ② the yield of the asphaltized product obtained by the method is low and is less than 30 percent; thirdly, the obtained asphaltized product has low yield and low quality, so the economical efficiency is not ideal.
Disclosure of Invention
As a result of intensive studies to solve the above problems, the present inventors have found that an asphalt-mineral composite material having a wide application field and application value can be prepared by using a high content of colloid and asphaltene components in a thick oil sludge and a clay mineral colloid contained therein to realize comprehensive utilization of waste resources, and the asphalt-mineral composite material is composed of a thick oil sludge, a softening point modifier and a brittle material, and is prepared by blending, melting, quenching and pulverizing, and specifically, the present invention provides the following aspects:
in a first aspect, the invention provides an asphalt-mineral composite material prepared from thick oil sludge, which is characterized by being prepared from the following components in parts by weight:
thick oil sludge: 40-80 parts;
softening point modifier: 10-30 parts;
brittle material: 5 to 20 parts of (A) a water-soluble polymer,
wherein,
the thick oil sludge is thick oil-containing sludge discharged by an oily sewage treatment combined station in the process of exploiting thick oil in the petroleum industry;
the brittle material is selected from: oil-soluble petroleum resin, lignite or mixtures thereof;
the softening point modifier is selected from: one or a mixture of a plurality of natural or artificial rosin resin, dehydrated fusel, high softening point asphalt, biochar, lignin and humic acid in any proportion, wherein,
the high-softening-point asphalt is asphalt with a softening point higher than 150 ℃;
the biochar is porous biochar processed by organic byproducts such as animal wastes, animal bones, plant roots and stems, wood chips or wheat straws and the like;
the dehydrated fusel is a product obtained by dehydrating aliphatic alcohols with carbon atom number more than 2;
the asphalt-mineral composite material is prepared by the following steps:
(1) weighing the thick oil sludge and the softening point regulator according to the weight ratio, uniformly mixing, and melting at the melting temperature of 80-200 ℃ after mixing;
(2) stopping heating after the mixture in the step (1) reaches a molten state, immediately adding the brittle material, melting the brittle material by using the residual temperature of the mixture, stirring the mixture until the mixture is a uniform fluid, and then suddenly cooling the mixture in normal-temperature water to obtain a composite material body;
(3) and (3) naturally drying the composite material body obtained in the step (2), and crushing the dried composite material body into powder particles with the particle size of 60-100 meshes.
In a second aspect, the invention provides the asphalt-mineral composite material prepared from the thick oil sludge, which is characterized by comprising the following components in parts by weight:
thick oil sludge: 55-75 parts;
softening point modifier: 15-22 parts;
brittle material: 10-15 parts;
the melting temperature in the step (1) is 100-150 ℃;
the crushing process in the step (3) is carried out in a blast cooling crusher;
the high-softening-point asphalt is asphalt with a softening point higher than 180 ℃.
In a third aspect, the present invention provides the asphalt-mineral composite material prepared from the thick oil sludge, wherein the high softening point asphalt is asphalt having a softening point of 190 to 260 ℃, and is selected from the following: one or more natural asphalts produced in Xinjiang, Sichuan, Iran and the like in any proportion.
In a fourth aspect, the present invention provides a method for preparing an asphalt-mineral composite material from thick oil sludge, which is characterized by comprising the following steps:
(1) weighing thick oil sludge and a softening point regulator, uniformly mixing, and melting at a melting temperature of 80-200 ℃ after mixing;
(2) stopping heating after the mixture in the step (1) reaches a molten state, immediately adding the brittle material, melting the brittle material by using the residual temperature of the mixture, stirring the mixture until the mixture is a uniform fluid, and then suddenly cooling the mixture in normal-temperature water to obtain a composite material body;
(3) naturally drying the composite material body obtained in the step (2), crushing the dried composite material body into powder particles with the particle size of 60-100 meshes,
wherein,
the thickened oil sludge is thickened oil-containing sludge discharged by an oily sewage treatment combined station in the process of exploiting thickened oil in the petroleum industry;
the brittle material is selected from: oil-soluble petroleum resin, lignite or mixtures thereof;
the softening point modifier is selected from: one or a mixture of a plurality of natural or artificial rosin resin, dehydrated fusel, high softening point asphalt, biochar, lignin and humic acid in any proportion, wherein,
the high-softening-point asphalt is asphalt with a softening point higher than 150 ℃;
the biochar is porous biochar processed by organic byproducts such as animal wastes, animal bones, plant roots and stems, wood chips or wheat straws and the like;
the dehydrated fusel is a product obtained by dehydrating aliphatic alcohols with carbon atom numbers more than two.
In a fifth aspect, the present invention provides the above method for preparing asphalt-mineral composite material from thick oil sludge, which is characterized in that,
the melting temperature in the step (1) is 100-150 ℃;
the crushing process in the step (3) is carried out in a blast cooling crusher;
the high-softening-point asphalt is asphalt with a softening point higher than 180 ℃.
In a sixth aspect, the present invention provides the method for preparing the asphalt-mineral composite material from the thick oil sludge, wherein the high softening point asphalt is asphalt with a softening point of 190 to 260 ℃ and is selected from the following: one or more natural asphalts produced in Xinjiang, Sichuan, Iran and the like in any proportion.
In a seventh aspect, the invention provides a method for preparing an asphalt-mineral composite material from thick oil sludge, which is characterized by comprising the following components in parts by weight:
thick oil sludge: 40-80 parts;
softening point modifier: 10-30 parts;
brittle material: 5-20 parts.
In an eighth aspect, the invention provides a method for preparing an asphalt-mineral composite material by using thick oil sludge, which is characterized by comprising the following components in parts by weight:
thick oil sludge: 55-75 parts;
softening point modifier: 15-22 parts;
brittle material: 10-15 parts.
In a ninth aspect, the invention provides the use of the asphalt-mineral composite material prepared by using the thick oil sludge for waterproof coiled materials, road asphalt and waste rubber regeneration.
In a tenth aspect, the invention provides a use of an asphalt-mineral composite material prepared from thick oil sludge for an anti-collapse agent for petroleum drilling.
According to the method for preparing the asphalt-mineral composite material by using the thick oil sludge and the asphalt-mineral composite material prepared by the method, the following beneficial effects are achieved:
(1) the method provided by the invention can effectively utilize the thick oil sludge generated in the processes of thick oil exploitation and thick oil-containing sewage treatment in the petroleum industry to prepare a product with practical value, realize harmless treatment of toxic and harmful substances and change waste into valuable;
(2) compared with the traditional treatment method, the method provided by the invention has the advantages of simple production process, convenient and easy implementation and strong practicability for treating the thick oil sludge, and can be popularized to the oil exploitation industry in a large scale;
(3) the method has high utilization rate of waste, realizes resource utilization production on the basis of harmlessness, reduces environmental pollution and creates certain economic value;
(4) the asphalt-mineral composite material prepared by the method provided by the invention contains about two thirds of oil-soluble hydrocarbon substances such as colloid, asphaltene and the like, contains one third of ultrafine inorganic mineral powder, and can be widely applied to waterproof coiled materials, road asphalt, waste rubber regeneration, petroleum drilling collapse prevention agents and the like;
(5) the thick oil sludge is prepared into the asphalt-mineral composite material with higher added value, so that the condition that the sludge is used alone or mixed with coal as fuel for low-value burning is avoided, and the toxic and harmful gas containing dioxin, which can cause serious environmental pollution, generated in the burning process is avoided.
Detailed Description
The invention is further explained or illustrated by the following examples. The examples provided should not be construed as limiting the scope of the invention.
The invention provides an asphalt-mineral composite material prepared from thick oil sludge, which comprises the following components in parts by weight:
thick oil sludge: 40-80 parts;
softening point modifier: 10-30 parts;
brittle material: 5 to 20 parts of (A) a water-soluble polymer,
preferably, the composition comprises the following components in parts by weight:
thick oil sludge: 55-75 parts;
softening point modifier: 15-22 parts;
brittle material: 10-15 parts.
Wherein,
the thick oil sludge is thick oil-containing sludge discharged by an oily sewage treatment combined station in the process of exploiting thick oil in the petroleum industry;
the brittle material is selected from: oil-soluble petroleum resins, for example, No. 10 oil-soluble resin, No. 16 oil-soluble resin, but the oil-soluble resins are not limited to the oil-soluble resin examples listed; lignite or mixtures thereof. The brittle material is added in the process of preparing the asphalt-mineral composite material, so that the prepared asphalt-mineral composite material can be crushed into a powder material convenient to use by an air-cooled crusher at normal temperature.
The softening point modifier is selected from: one or a mixture of more of natural or artificial rosin resin, dehydrated fusel, high-softening-point asphalt, biochar, lignin and humic acid in any proportion.
The asphalt-mineral composite material prepared from the thick oil sludge with the high softening point can present the characteristics of a solid composite material similar to asphalt at normal temperature, but the asphalt-mineral composite material prepared from the thick oil sludge with the low softening point does not have the characteristics, however, the thick oil sludge used as a raw material of the asphalt-mineral composite material has a large amount of colloid and asphaltene components with lower softening points, so that the high-softening-point material is required to be added to increase the softening point of the thick oil sludge so as to prepare the required asphalt-mineral composite material. The selected high-softening-point asphalt is asphalt with a softening point higher than 150 ℃, preferably higher than 180 ℃, and more preferably 190-260 ℃.
The biochar is brittle organic carbon, and the addition of the biochar into the thick oil sludge is beneficial to improving the softening point of the prepared asphalt-mineral composite material and increasing the brittleness of the prepared asphalt-mineral composite material, so that the subsequent crushing of the asphalt-mineral composite material is facilitated. The preferred biochar of the invention is porous biochar processed from organic by-products such as animal waste, animal bones, plant rhizomes, wood chips or wheat straws.
The dehydrated fusel alcohol is a polyol prepared by mixing industrial byproducts of biological alcohol, and the main components of the dehydrated fusel alcohol are dihydric alcohol, trihydric alcohol and low molecular polymers thereof. Under the condition of high temperature, rich hydroxyl contained in fusel and carboxyl, amino and the like contained in colloid and asphaltene are subjected to esterification and (or) crosslinking chemical reaction to generate reticular condensed ring macromolecules with higher molecular weight, and the condensed ring macromolecules can enhance the adhesive property and toughness of the colloid and the asphaltene, improve the viscoelasticity of the prepared composite material and enable the composite material to have the visco-elastic property similar to that of the asphalt really. The anhydrofusel selected in the present invention is a product obtained by dehydrating aliphatic alcohol having more than 2 carbon atoms, such as a mixture mainly composed of ethylene glycol, propylene glycol, butylene glycol, glycerol and oligomers thereof, but is not limited to the exemplified anhydrofusel.
The invention provides a method for preparing an asphalt-mineral composite material by using thick oil sludge, which specifically comprises the following steps:
(1) weighing thick oil sludge and a softening point regulator, uniformly mixing, and melting at a melting temperature of 80-200 ℃ after mixing;
(2) stopping heating after the mixture in the step (1) reaches a molten state, immediately adding the brittle material, melting the brittle material by using the residual temperature of the mixture, stirring the mixture until the mixture is a uniform fluid, and then suddenly cooling the mixture in normal-temperature water to obtain a composite material body;
(3) and (3) naturally drying the composite material body obtained in the step (2), and crushing the dried composite material body into powder particles with the particle size of 60-100 meshes.
The thick oil sludge is waste produced in thick oil exploitation in the petroleum industry, is solid or semi-solid at normal temperature, contains a large amount of colloid and asphaltene substances, has the characteristics of high solidification point, high viscosity, high density, small oil-water density difference and the like, can be mutually fused with a softening point regulator to form a homogeneous mixture when the temperature is higher than the melting point of the thick oil sludge, namely higher than 80 ℃, and the brittle material is selected from oil-soluble petroleum resin, lignite or a mixture thereof, has a lower melting point than the thick oil sludge and the softening point regulator, so that the brittle material can be added after the first two components are uniformly fused and mixed, and the fusion of the brittle material can be realized by means of the rest heat, thereby saving the energy cost; however, the melting temperature is not too high, and when the temperature is higher than 200 ℃, the thick oil sludge can generate carbonization reaction, thereby causing the reduction of the product performance of the composite material.
The composite bodies prepared by the present invention should undergo a quenching process when discharged from the reactor. The quenching process can quickly solidify the liquid composite material body after melting and mixing into a solid composite material, thereby being beneficial to the operation of the subsequent crushing step and improving the production efficiency; meanwhile, in the quenching process, as the water vapor wrapped in the molten liquid composite material cannot overflow in time to form a porous structure in the solid composite material, the porosity and brittleness of the composite material are improved, the prepared asphalt-mineral composite material is easier to crush, and the asphalt-mineral composite powder material suitable for various working conditions can be conveniently prepared.
The invention also provides the application of the asphalt-mineral composite material prepared based on the method in waterproof coiled materials, road asphalt, waste rubber regeneration and petroleum drilling anti-collapse agents.
The method for preparing the asphalt-mineral composite material by using the thick oil sludge and the asphalt mineral composite material prepared by the method have the following advantages:
firstly, the method provided by the invention can effectively utilize the thick oil sludge generated in the processes of thick oil exploitation and thick oil-containing sewage treatment in the petroleum industry to prepare a product with practical value, realize harmless treatment of toxic and harmful substances and change waste into valuable;
secondly, compared with the traditional treatment method, the method provided by the invention has the advantages of simple production process, convenient and easy implementation and strong practicability for treating the thick oil sludge, and can be popularized to the oil exploitation industry in a large scale;
thirdly, the method has high utilization rate of waste, realizes resource utilization production on the basis of harmlessness, reduces environmental pollution and creates certain economic value;
fourthly, the asphalt-mineral composite material prepared by the method provided by the invention contains about two thirds of oil-soluble hydrocarbon substances such as colloid, asphaltene and the like, contains one third of ultrafine inorganic mineral powder, and can be widely applied to waterproof coiled materials, road asphalt, waste rubber regeneration, petroleum drilling collapse prevention agents and the like;
fifthly, the thick oil sludge is prepared into the asphalt-mineral composite material with higher added value, so that the condition that the sludge is used alone or mixed with coal as fuel for low-value burning is avoided, and toxic and harmful gas containing dioxin causing serious environmental pollution can be generated in the burning process, so that the thick oil sludge is fully utilized as a precious resource, and the purposes of changing waste into valuables and realizing clean recycling of the resource are achieved.
Examples
High softening point bitumen used in example 1: the natural asphalt produced by 137 groups of natural asphalt ore by 7 soldiers in the military sector for production and construction in Xinjiang has the oil solubility of 96 percent, the softening point (by a ring-and-ball method) of 160-190 ℃ and the density (at 25 ℃) of 1.04g/cm3The flash point of the opening is more than 350 ℃, and the contents of main components are 2-3% of saturated hydrocarbon, 4-11% of aromatic hydrocarbon, 32-64% of asphaltene and 30-54% of colloid;
oil-soluble resin used in example 1: the softening point of the Zibo zibang petroleum resin No. 10C 9 produced by a resin factory is 80-130 ℃, and the oil solubility is 98%;
rosin resin used in example 2: pro12991816 rosin resin produced by Qinghuizhihua products Limited in the North district of Tianjin, the softening point of which is 100-120 ℃;
lignite used in example 2: brown coal powder produced by Nikoku humic acid science and technology Limited liability company of inner Mongolia Huo coal, the humic acid content is 70%;
anhydrofusel used in example 3: dehydrated fusel oil produced in Shenyang Sujie chemical plant contains ethylene glycol, propylene glycol, butanediol, glycerol and their oligomer mixture as main ingredients;
oil-soluble resin used in example 3: the softening point of 16 # C9 petroleum resin produced by Zibo Zibang resin factory is 80-130 ℃, and the oil solubility is 95%;
mavron resin used in example 4: the ancient Mallon resin produced by Shenzhen Jitian chemical industry Limited has a softening point of 70-105 ℃ and an oil solubility of 98%;
plant asphalt used in example 4: VGA-VA270 plant asphalt produced by Shanghai Dacheng company has a softening point of 80 ℃, a kinematic viscosity (60 ℃) of more than or equal to 230 pas, a volatility (163 ℃ multiplied by 3h) of less than or equal to 1 and a density (25 ℃) =1.268g/cm3The water content is less than or equal to 1 percent.
The thick oil sludge used in the following examples is a homogenized and dehydrated thick oil sludge sample from Liaohe oilfield Hua oil group thick oil sludge treatment plant. However, it will be readily appreciated that the technique of the present invention is equally applicable to thick oil sludge produced by other thick oil fields of similar composition. Example 1
(1) Weighing 240kg of thick oil sludge and 80kg of natural asphalt with high softening point, uniformly mixing, and melting at the high temperature of 200 ℃;
(2) stopping heating after melting for 60 minutes, adding 40kg of No. 10 oil-soluble resin serving as a brittle material, melting the No. 10 oil-soluble resin by using the waste heat of high-temperature thick oil sludge, stirring to obtain a uniform fluid, and then suddenly cooling in normal-temperature clear water to obtain a composite material body;
(3) and (3) naturally drying the composite material body prepared in the step (2) in a cool and ventilated place, and then crushing the composite material body into powder particles with the particle size of 100 meshes by using a blast cooling crusher to obtain the sample of the example 1.
Example 2
(1) Weighing 240kg of thick oil sludge and 100kg of rosin resin, and melting at the high temperature of 140 ℃;
(2) stopping heating after 1 hour of melting, adding 80kg of lignite serving as a brittle material, melting the lignite by using the waste heat of high-temperature thick oil sludge, stirring to obtain a uniform fluid, and then suddenly cooling in normal-temperature clean water to obtain a composite material body;
(3) the composite material precursor obtained in step (2) was naturally dried in a cool and ventilated place, and then pulverized by a forced air cooling pulverizer to powder particles having a particle size of 80 mesh, to obtain a sample of example 2.
Example 3
(1) Weighing 240kg of thick oil sludge and 60kg of dehydrated fusel, and melting at the high temperature of 120 ℃;
(2) stopping heating after melting for 40 minutes, adding 60kg of No. 16 oil-soluble resin as a brittle material, melting the No. 16 oil-soluble resin by using the waste heat of high-temperature thick oil sludge, stirring to uniform fluid, and then suddenly cooling in normal-temperature clear water to obtain a composite material body;
(3) and (3) naturally drying the composite material body prepared in the step (2) in a cool and ventilated place, and then crushing the composite material body into powder particles with the particle size of 60 meshes by using a blast cooling crusher to obtain the sample of the example 3.
Example 4
(1) Weighing 240kg of thick oil sludge and 60kg of mavulong resin, and melting at the high temperature of 100 ℃;
(2) stopping heating after melting for 1 hour, adding 100kg of plant asphalt, melting the plant asphalt by using the waste heat of the high-temperature thick oil sludge, stirring to obtain a uniform fluid, and suddenly cooling in normal-temperature clear water to obtain a composite material body;
(3) the composite material precursor prepared in the step (2) was naturally dried in a cool and ventilated place, and then pulverized by a forced air cooling pulverizer to powder particles having a particle size of 100 mesh, to obtain a sample of example 4.
Examples of the experiments
The samples used in this example were all selected from the examples 1-4 above.
Experimental example 1 fineness measurement
Weighing 50.00g of a sample, placing the sample in a 30-mesh standard sieve, quickly vibrating the standard sieve until the sample does not leak, weighing the mass of the residue on the sieve, and calculating the fineness according to the following formula:
in the formula: s-fineness (%);
m 1-amount of rejects (g);
m-weigh the sample mass (g).
Experimental example 2 oil solubility measurement
(1) Placing 0.2-0.3 g of absorbent cotton, a piece of lens wiping paper and a section of line in a weighing bottle, and drying at 105 ℃ until the weight is constant for later use;
(2) folding the lens wiping paper in the step (1) in half, flatly paving the folded lens wiping paper on weighing paper, then uniformly paving absorbent cotton in the middle of the lens wiping paper, weighing 0.5g of a sample which is ground and sieved by a standard sieve with the side length of a sieve pore of 0.28mm, and placing the sample in the center of the absorbent cotton;
(3) tightly wrapping the sample in the step (2) with absorbent cotton, tightly wrapping the cotton with a piece of mirror wiping paper, and finally wrapping the sample with the thread in the step (1), wherein the sample cannot leak outside in the sample wrapping process, the sample cannot be obviously seen in the wrapped sample bag, and the sample bag is placed into a sample cup in an extractor, and the sample cup is hung below a micro condensation pipe in the extractor;
(4) injecting 250mL of carbon tetrachloride (boiling point 76.8 ℃) into the extractor, putting the extractor into an electric heating sleeve, heating to 80 ℃ and keeping a boiling state until effluent liquid is colorless;
(5) taking out the sample cup, placing the paper roll wrapped with the sample in a drying oven, drying at 105 ℃ for 2h, taking out, placing in a dryer, cooling at normal temperature for 30min, and weighing;
(6) the oil solubility was calculated as follows:
in the formula: wo-oil solubility (%);
m7-sample mass (g);
m8-absorbent cotton, lens wiping paper and sample mass (g);
m9absorbent cotton, lens wiping paper and the amount of residue (g).
Experimental example 3 softening Point measurement
The sample is burned at 280 ℃ for 30min and then the softening point is measured according to GB/T4507-84 (namely, a ring and ball method).
The samples used in this experimental example were prepared in examples 1 to 4.
The results of the physical and chemical property tests are shown in the following table 1:
table 1 results of quality testing of physical and chemical properties of samples of examples
The asphalt-mineral composite material prepared by the method has the characteristics of controllable granularity, higher oil solubility, lower softening point, convenient processing and use and the like, is suitable for being used as an asphalt substitute in various fields such as waterproof coiled materials, road asphalt modification, waste rubber powder regeneration softening, oil field drilling fluid chemicals and the like, and has higher cost performance.
The invention has been described in detail with reference to specific embodiments and illustrative examples, but the description is not intended to be construed in a limiting sense. Those skilled in the art will appreciate that various equivalent substitutions, modifications or improvements may be made to the technical solution of the present invention and its embodiments without departing from the spirit and scope of the present invention, which fall within the scope of the present invention. The scope of the invention is defined by the appended claims.
Claims (14)
1. The asphalt-mineral composite material prepared from the thick oil sludge is characterized by being prepared from the following components in parts by weight:
thick oil sludge: 40-80 parts;
softening point modifier: 10-30 parts;
brittle material: 5 to 20 parts of (A) a water-soluble polymer,
wherein,
the thick oil sludge is thick oil-containing sludge discharged by an oily sewage treatment combined station in the process of exploiting thick oil in the petroleum industry;
the brittle material is selected from: oil-soluble petroleum resin, lignite or mixtures thereof;
the softening point modifier is selected from: one or a mixture of a plurality of natural or artificial rosin resin, dehydrated fusel, high softening point asphalt, biochar, lignin and humic acid in any proportion, wherein,
the high-softening-point asphalt is asphalt with a softening point higher than 150 ℃;
the biochar is porous biochar processed by organic byproducts;
the dehydrated fusel is a product obtained by dehydrating aliphatic alcohols with carbon atom number more than 2;
the asphalt-mineral composite material is prepared by the following method:
(1) weighing the thick oil sludge and the softening point regulator according to the weight ratio, uniformly mixing, and melting at the melting temperature of 80-200 ℃ after mixing;
(2) stopping heating after the mixture in the step (1) reaches a molten state, immediately adding the brittle material, melting the brittle material by using the residual temperature of the mixture, stirring the mixture until the mixture is a uniform fluid, and then suddenly cooling the mixture in normal-temperature water to obtain a composite material body;
(3) and (3) naturally drying the composite material body obtained in the step (2), and crushing the dried composite material body into powder particles with the particle size of 60-100 meshes.
2. The asphalt-mineral composite material prepared from thick oil sludge as claimed in claim 1, wherein the organic by-product is selected from animal wastes, animal bones, plant roots, wood chips or wheat straw.
3. The asphalt-mineral composite material prepared by using the thick oil sludge as claimed in claim 1 or 2, which is characterized by comprising the following components in parts by weight:
thick oil sludge: 55-75 parts;
softening point modifier: 15-22 parts;
brittle material: 10-15 parts;
the melting temperature in the step (1) is 100-150 ℃;
the crushing process in the step (3) is carried out in a blast cooling crusher;
the high-softening-point asphalt is asphalt with a softening point higher than 180 ℃.
4. The asphalt-mineral composite material prepared by using the thick oil sludge as claimed in claim 1 or 2, wherein the high softening point asphalt is asphalt with a softening point of 190-260 ℃.
5. The asphalt-mineral composite material prepared from thick oil sludge as claimed in claim 4, wherein the high softening point asphalt is selected from the group consisting of: one or a mixture of more of natural asphalts produced in Xinjiang, Sichuan and Iran in any proportion.
6. A method for preparing asphalt-mineral composite material by using thick oil sludge is characterized by comprising the following steps:
(1) weighing thick oil sludge and a softening point regulator, uniformly mixing, and melting at a melting temperature of 80-200 ℃ after mixing;
(2) stopping heating after the mixture in the step (1) reaches a molten state, immediately adding the brittle material, melting the brittle material by using the residual temperature of the mixture, stirring the mixture until the mixture is a uniform fluid, and then suddenly cooling the mixture in normal-temperature water to obtain a composite material body;
(3) naturally drying the composite material body obtained in the step (2), crushing the dried composite material body into powder particles with the particle size of 60-100 meshes,
wherein,
the thick oil sludge is thick oil-containing sludge discharged by an oily sewage treatment combined station in the process of exploiting thick oil in the petroleum industry;
the brittle material is selected from: oil-soluble petroleum resin, lignite or mixtures thereof;
the softening point modifier is selected from: one or a mixture of a plurality of natural or artificial rosin resin, dehydrated fusel, high softening point asphalt, biochar, lignin and humic acid in any proportion, wherein,
the high-softening-point asphalt is asphalt with a softening point higher than 150 ℃;
the biochar is porous biochar processed by organic byproducts;
the dehydrated fusel is a product obtained by dehydrating aliphatic alcohols with carbon atom number more than 2.
7. The method for preparing asphalt-mineral composite material from thick oil sludge as claimed in claim 6, wherein the organic by-product is selected from animal wastes, animal bones, plant roots, wood chips or wheat straw.
8. The method for preparing asphalt-mineral composite material using thick oil sludge as claimed in claim 6 or 7,
the melting temperature in the step (1) is 100-150 ℃;
the crushing process in the step (3) is carried out in a blast cooling crusher;
the high-softening-point asphalt is asphalt with a softening point higher than 180 ℃.
9. The method for preparing the asphalt-mineral composite material by using the thick oil sludge as claimed in claim 6 or 7, wherein the high softening point asphalt is asphalt with a softening point of 190-260 ℃.
10. The method of claim 9, wherein the high softening point asphalt is selected from the group consisting of: one or a mixture of more of natural asphalts produced in Xinjiang, Sichuan and Iran in any proportion.
11. The method for preparing the asphalt-mineral composite material by using the thick oil sludge as claimed in claim 6 or 7, which is characterized by comprising the following components in parts by weight:
thick oil sludge: 40-80 parts;
softening point modifier: 10-30 parts;
brittle material: 5-20 parts.
12. The method for preparing the asphalt-mineral composite material by using the thick oil sludge as claimed in claim 6 or 7, which is characterized by comprising the following components in parts by weight:
thick oil sludge: 55-75 parts;
softening point modifier: 15-22 parts;
brittle material: 10-15 parts.
13. Use of the asphalt-mineral composite material prepared from the thick oil sludge according to any one of claims 1 to 5 for recycling waterproof coiled materials, road asphalt and waste rubber.
14. Use of the asphalt-mineral composite material prepared from the thick oil sludge according to any one of claims 1 to 5 as an anti-sloughing agent for petroleum drilling.
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| 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 |
| 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 |
| 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 |
| 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 |
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| CN101045600A (en) * | 2006-03-29 | 2007-10-03 | 中国科学院沈阳应用生态研究所 | Treatment method of oil-contained slag asphalt |
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