A kind of no alveolitoid cleaning agent and the preparation method and application thereof
Technical field
The invention belongs to petroleum drilling technology fields, and in particular to a kind of no alveolitoid cleaning agent and preparation method thereof with answer
With.
Background technique
Currently, with being continuously increased for deep-well, high temperature well and shale gas well, oil base bores in oil/gas well exploration and development
The application of well liquid is also increasing, although the application of oil base drilling fluid greatly reduces the various complicated feelings in drilling process
Condition, but it is also easily adhered on down-hole casing, oil pipe and tool string, not easy-clear;To the multistage bridge plug to completion practice
It sets, electrical measurement, perforating job and oil gas adopt defeated operation and causes great limitation.Usual situation is adhered to casing wall or oil pipe
The oil base drilling fluid residue of wall will cause bridge plug set failure, electrical measurement tool and perforating gun decentralization less than purpose depth and
The case where causing oil gas to adopt oil transportation blockage.In order to guarantee completion practice and adopt going on smoothly for defeated operation, it is necessary to underground
Oil base drilling fluid residue in casing and oil pipe is cleaned.
Oil base drilling fluid is the stable water-in-oil emulsion fluid of a kind of complicated components, colloform texture, and component generally comprises
Adhere to the strong dissolved organic colloids of polarity, oily phase, water phase, heavy weight additive etc..Therefore to the oil base drilling fluid residue for remaining in underground
The following aspects must be considered when cleaning: 1, cleaning agent has good dissolution and dispersibility to oil base drilling fluid;2, it cleans
Agent has good heat-resisting property, still has good cleaning ability in shaft bottom high temperature to meet;3, have and centainly take grittiness
Can, the high density solid formation that shaft bottom washes out is carried out shaft bottom to meet;4, when to cleaning oil pipe, cleaning agent must be considered
The case where payzone can be entered, not will cause Shale Hydration expansion, causes after guaranteeing that cleaning agent enters water-sensitive shale payzone
Hydrocarbon stratum channel blockage, cleaning solution must have good shale inhibition energy;5, it when cleaning oil pipe, returns and clears washing lotion as existed
A large amount of foams, it will usually cause ground to adopt the shut-down of transfer device, to influence to adopt defeated operation;Therefore, cleaning agent must be still.6, clear
Corrosivity should be not present to metal sleeve, oil pipe in lotion.7, flash-point is higher, to guarantee the safety of field operation.8, cleaning agent group
Sorting in application process impacts environment to avoid cleaning solution with environmental protection is answered.
Chinese patent CN104152127A discloses a kind of oil field multifuctional cleaning agent and its preparation method and application, by
Compound nonylphenol polyoxyethylene ether activating agent 0.2%-1.0%, compound quaternary ammonium salt cationic active agent chloride 0.2%-
1.0%;Compound restrainer 0%-1.0%, compound Fe ion chelating agent 0%-1.0%, organic carboxylic ester 0%-10.0%,
Remaining is water composition, this cleaning agent is under the conditions of 60 DEG C -80 DEG C to CaCO3、Fe2O3, FeS inorganic chemistry dirt have good acid
Xie Rong has dispersion and melting except effect, to grease, wax dirt and heavy oil stain, has killing effect to oil field mushroom, to glutinous dirt
Play the role of removing, be suitable for oil extraction in oil field well shaft, gathering line, water-oil separating settling tank, flocculating setting tank, oil storage tank,
The cleaning of the equipment such as sewage storage cylinder.The invention cleaning agent is the hydrotrope of surfactant and other auxiliary agents, but is applying
Surfactant can generate the influence that a large amount of foams adopt ground oil gas defeated supercharging equipment in the process, return row in later period cleaning solution
In the process, in auxiliary agent there is certain influence to environment in chloride, while also be not directed to wellbore bottom high density solid formation
Carrying.
Chinese patent CN103589412A discloses a kind of shale gas exploitation oil base drilling fluid mud cake cleaning solution, belongs to petroleum drilling
Well engineering chemistry agent technical field, consisting of cleaning agent, heavy weight additive, water;The weight percent of each component are as follows: cleaning agent
10%-30%, heavy weight additive 0%-60%, water surplus, cleaning agent are made of nonionic surfactant and mutual solvent, nonionic table
The weight ratio of face activating agent and mutual solvent is 1:9-9:1;Nonionic surfactant is aliphatic acid polyethenoxy ether, polyoxyethylene
Aliphatic ester, polyoxypropylene aliphatic ester etc., mutual solvent are methanol, ethyl alcohol, isopropanol etc., and heavy weight additive is ultra-fine Iron Ore Powder powder
End, density 4.90-5.20g/cm3.The invention, which not can solve, to be generated a large amount of foams in application process ground oil gas is adopted
The influence of defeated supercharging equipment, while being confined to be used as the flushing of oil base drilling fluid on formation rock when cementing the well, it does not consider
The anti-corrosion of metal surface when being cleaned in casing and in oil pipe, also not in view of cleaning solution enters shale layer of oil gas production to payzone
The problems such as gas channel caused by hydration swelling blocks, while being also unable to satisfy the still of cleaning oil pipe in gas production production operation and wanting
It asks;Heavy weight additive solid phase will cause gas channel blocking in cleaning solution.
Oil base drilling fluid cleaning agent in the prior art, mostly well cementation irrigation, working interface is mostly formation rock, not
Once it was related to the cleaning and production tube anti-corrosion of casing, oil base drilling fluid residue on tubing wall metal interface;Existing oil base bores
Well liquid cleaning agent group is divided into surfactant or organic solvent, and a large amount of foams are easy to produce in cleaning process;Without for production oil
The still cleaning agent of pipe washing and cleaning operation, aqueous surfactant generate a large amount of foam after reducing interfacial tension, seriously affect gas production work
The normal work of industry ground gas collecting equipment;Existing cleaning agent be not related to the carrying of greasy dirt middle-high density solid phase;It is not related to oil
The protection of pipe shale payzone strong to water sensitivity when cleaning.
For these reasons, the present invention is specifically proposed.
Summary of the invention
In order to solve problem above of the existing technology, the present invention provides a kind of no alveolitoid cleaning agent and its preparation sides
Method and application.Of the invention realizes efficiently still effect without alveolitoid cleaning agent, solves because a large amount of in live use process
Gas production operation can not continue the problem of carrying out caused by foam adopts the influence that defeated supercharging equipment works normally to oil gas, clean
While focus on down-hole casing, oil pipe anti-corrosion protection, prolong its service life, cleaning while be also able to satisfy shaft bottom wash out
The carrying of high density solid formation, the strong rejection capability of cleaning agent of the invention are more conducive to the protection of water-sensitive shale oil-gas Layer, each group
Divide environmental protection, environmental sound.
The first object of the present invention, provides a kind of no alveolitoid cleaning agent, and the cleaning agent includes coconut oil diethanol
Amide, positive decyl glucoside, dimethyl silicone polymer, oleic acid base hydroxyethyl imidazole quinoline, isothiazolinone, potassium acetate, xanthan
Glue, paraffin oil and water.
It is of the invention that there is the effect of inhibition corrosion-resistant without the oleic acid base hydroxyethyl imidazole quinoline being added in alveolitoid cleaning agent, it can be with
Cleaning while focus on down-hole casing, oil pipe anti-corrosion protection, prolong the service life, isothiazolinone have sterilization work
With preventing suspending agent xanthan gum from biodegrade occurring in use, it is ensured that the viscosity that xanthan gum can be improved cleaning agent is
Precipitation solid phase in cleaning process provides suspending power, meets the carrying that shaft bottom washes out high density solid formation;Meanwhile xanthan gum
Space net structure can make prepared cleaning agent oil-in-water emulsion type product more stable, in addition, cleaning agent of the present invention is water
Oil-in cleaning agent, wherein oil-phase component paraffin oil has good dispersion and solubilising power, tool to oil base drilling fluid residue
Have the characteristics that efficiently still, while the dimethyl silicone polymer in component also plays good foam-inhibiting effect, is using this hair
When bright cleaning agent carries out the residue of cleaning oil base drilling fluid, returns and clear washing lotion and will not generate foam, can avoid a large amount of foams
The shut-down of ground gas production supercharging equipment is caused, to guarantee to adopt the normal operation of defeated operation;The potassium ion of potassium acetate can in the present invention
Inhibit the dispersion of layer of oil gas production shale hydration, effectively prevent blocking of the aquation dispersed shale to gas channel, and potassium acetate is easy
Degradation organic salt, returning drain not can cause environmental pollution;Each component environmental protection, it is nontoxic, harmless, non-corrosive.
Further, according to parts by weight, the cleaning agent includes lauric acid amide of ethanol 5-10 parts by weight, positive decyl
Glucoside 5-15 parts by weight, dimethyl silicone polymer 0.3-1 parts by weight, oleic acid base hydroxyethyl imidazole quinoline 1-3 parts by weight, different thiophene
Oxazoline ketone 0.05-0.4 parts by weight, potassium acetate 7-11 parts by weight, xanthan gum 0.3-0.4 parts by weight, paraffin oil 30-55 parts by weight and
Water 30-40 parts by weight.
The applicant is had clear by a large amount of test discovery using the cleaning agent that each raw material of aforementioned proportion is prepared
It washes that excellent effect, stability is more preferable, the more low advantage of blistering rate, therefore is only carried out using the raw material of special ratios of the invention
Cleaning agent made of compounding also has better economic promotional value while meeting Oil Field application technology and requiring,
Component is too low not to be able to satisfy that field use requires, excessively high product itself mobility that will affect causes the inconvenient of application and increase to answer
Use cost.
Further, according to parts by weight, the cleaning agent includes 7.5 parts by weight of lauric acid amide of ethanol, positive decyl
10 parts by weight of glucoside, 0.6 parts by weight of dimethyl silicone polymer, 2 parts by weight of oleic acid base hydroxyethyl imidazole quinoline, isothiazolinone
0.22 parts by weight, 9 parts by weight of potassium acetate, 35 parts by weight of 0.35 parts by weight of xanthan gum, 42 parts by weight of paraffin oil and water.
The second object of the present invention provides the preparation method without alveolitoid cleaning agent described in one kind, the preparation method
Include the following steps:
(1) it is weighed according to the weight of each component spare;
(2) weighed water is put into stirred tank, weighed potassium acetate is then added, stirs evenly, sufficiently dissolved, obtain
Acetic acid aqueous solutions of potassium is spare;
(3) under stirring conditions, weighed xanthan gum is added in acetic acid aqueous solutions of potassium, and heating stirring kettle;
(4) solution that step (3) are heated is put into circulation shear kettle and is sheared, obtain homogeneous liquid, close shearing
Pump;
(5) homogeneous liquid is put into stirred tank, under stirring, is sequentially added into stirred tank spare
Lauric acid amide of ethanol, positive decyl glucoside, dimethyl silicone polymer, oleic acid base hydroxyethyl imidazole quinoline, isothiazolinone,
It is sufficiently stirred;
(6) under stirring conditions, the uniform speed slow into stirred tank is pumped by circulation shear and paraffin oil is added, obtained described
Without alveolitoid cleaning agent.
Further, heating temperature is 40-50 DEG C in step (3).
Further, homogeneous liquid described in step (4) is at 30 DEG C, apparent viscosity 35-50mpas.
Further, step (4) medium shear rate is 150-200s-1。
Further, stirring rate is 180-200rpm, mixing time 25-35min in step (5).
Further, step (6) medium shear rate is 160-180s-1, the shear agitation time is 1.8-2.2 hours.
Preparation without alveolitoid cleaning agent of the invention needs to carry out stringent control, such as mixing time, and stirring rate is cut
Cutting speed rate, shear time, heating temperature are all that the applicant increases by a large amount of experiment and scheduling and planning discovery, heating temperature
Too many power consumption and time are not may require that 40 DEG C -50 DEG C, and xanthan gum is easier to be sheared dispersion in this temperature range
Uniformly, it is not likely to produce agglomeration, the end properties of acquisition are more stable, and temperature is too low to be unfavorable for that shearing dispersion, excessively high it will cause mistakes
Multiple-energy-source and time loss;Apparent viscosity control is to measure every batch of products obtained therefrom uniform quality between 35-50mPa.S
And meet field use and take sand requirement, it is too low to be unfavorable for taking sand, excessively high mobility when will affect products application;Shear rate,
Stirring rate and shear time are obtained according to production equipment situation and cleaning agent production requirement debugging, too low to will affect product
Quality, the excessively high operation for being unfavorable for equipment and service life obtained;And pass through cleaning agent blistering rate prepared by the above control condition
It is low, stability is good and meets the production of safe and efficient batch.
The third object of the present invention provides described in one kind without alveolitoid cleaning agent in cleaning oil base drilling fluid residue
Application.
Compared with prior art, the invention has the benefit that
(1) oleic acid base hydroxyethyl imidazole quinoline has the effect of inhibition corrosion-resistant in cleaning agent of the invention, can be in cleaning
Simultaneously focus on down-hole casing, oil pipe anti-corrosion protection, prolong the service life, isothiazolinone have the function of sterilize, xanthan gum
It can be improved the viscosity of cleaning agent and provide suspending power for the precipitation solid phase in cleaning process, meet shaft bottom and wash out high density solid phase
The carrying of object;Meanwhile the space net structure of xanthan gum can make prepared oil-in-water type rinse product more stable, separately
Outside, cleaning agent of the present invention is oil-in-water type cleaning agent, and wherein oil-phase component paraffin oil has oil base drilling fluid residue good
Dispersion and solubilising power, have the characteristics that efficiently it is still, while the dimethyl silicone polymer in component also play it is good
Foam-inhibiting effect is returned when being carried out the residue of cleaning oil base drilling fluid using cleaning agent of the invention and clears washing lotion and will not generate
Foam can avoid the shut-down that a large amount of foams cause ground gas production supercharging equipment, to guarantee to adopt the normal operation of defeated operation;The present invention
The potassium ion of middle potassium acetate can inhibit the dispersion of layer of oil gas production shale hydration, effectively prevent aquation dispersed shale to gas channel
Blocking, and potassium acetate is degradable organic salt, returning drain not can cause environmental pollution;Each component environmental protection, nontoxic, harmless, nothing
Corrosivity;
(2) cleaning agent of the invention is soluble easily in water, and acid and alkali-resistance, demulsification, suspension, dispersion, solubilising and wetting ability are strong, to group
Divide complexity, the stable oil base drilling fluid of colloform texture and various complex component greasy dirts can play fabulous cleaning effect, bore simultaneously
The rubber and cement plug generated during well, cleaning agent of the invention can also be carried out ground;
(3) cleaning agent high temperature resistant of the invention, can reach 150 DEG C or more, the construction for the deep-well washing and cleaning operation that can reach a high temperature
It is required that;
(4) there is good rolling action for the greasy dirt middle-high density solid formation of oil base drilling fluid, in cleaning greasy dirt
Pit shaft is also cleaned simultaneously, the high density solid formation after avoiding cleaning continues to remain on casing, causes other multiple in oil pipe
Miscellaneous situation;
(5) cleaning agent of the invention will not damage water-sensitive shale layer of oil gas production after entering layer of oil gas production;
(6) preparation method of cleaning agent of the invention is simple, can be mass produced.
Specific embodiment
To make the object, technical solutions and advantages of the present invention clearer, technical solution of the present invention will be carried out below
Detailed description.Obviously, described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.Base
Embodiment in the present invention, those of ordinary skill in the art are obtained all without making creative work
Other embodiment belongs to the range that the present invention is protected.
Embodiment 1
A kind of no alveolitoid cleaning agent of the present embodiment, the cleaning agent include lauric acid amide of ethanol 5kg, positive decyl Portugal
Polyglycoside 5kg, dimethyl silicone polymer 0.3kg, oleic acid base hydroxyethyl imidazole quinoline 1kg, isothiazolinone 0.05kg, potassium acetate
7kg, xanthan gum 0.3kg, paraffin oil 30kg and water 30kg.
The preparation method without alveolitoid cleaning agent of the present embodiment, includes the following steps:
(1) it is weighed according to the weight of each component spare;
(2) weighed water is put into stirred tank, weighed potassium acetate is then added, stirs evenly, sufficiently dissolved, obtain
Acetic acid aqueous solutions of potassium is spare;
(3) under stirring conditions, weighed xanthan gum is added in acetic acid aqueous solutions of potassium, and heating stirring kettle, is added
Hot temperature is to 40 DEG C;
(4) solution that step (3) are heated is put into circulation shear kettle and is sheared, shear rate 150s-1, obtain
Matter liquid, the homogeneous liquid is at 30 DEG C, when apparent viscosity is 35mpas, closes shear pump;
(5) homogeneous liquid is put into stirred tank, under stirring, is sequentially added into stirred tank spare
Lauric acid amide of ethanol, positive decyl glucoside, dimethyl silicone polymer, oleic acid base hydroxyethyl imidazole quinoline, isothiazolinone,
It is sufficiently stirred, stirring rate 180rpm, mixing time 25min;
(6) under stirring conditions, the uniform speed slow into stirred tank is pumped by circulation shear and paraffin oil, shear rate is added
For 160s-1, the shear agitation time is 1.8 hours, is obtained described without alveolitoid cleaning agent.
Embodiment 2
A kind of no alveolitoid cleaning agent of the present embodiment, the cleaning agent include lauric acid amide of ethanol 7.5kg, the positive last of the ten Heavenly stems
Base glucoside 10kg, dimethyl silicone polymer 0.6kg, oleic acid base hydroxyethyl imidazole quinoline 2kg, isothiazolinone 0.22kg, vinegar
Sour potassium 9kg, xanthan gum 0.35kg, paraffin oil 42kg and water 35kg.
The preparation method without alveolitoid cleaning agent of the present embodiment, includes the following steps:
(1) it is weighed according to the weight of each component spare;
(2) weighed water is put into stirred tank, weighed potassium acetate is then added, stirs evenly, sufficiently dissolved, obtain
Acetic acid aqueous solutions of potassium is spare;
(3) under stirring conditions, weighed xanthan gum is added in acetic acid aqueous solutions of potassium, and heating stirring kettle, is added
Hot temperature is to 45 DEG C;
(4) solution that step (3) are heated is put into circulation shear kettle and is sheared, shear rate 175s-1, obtain
Matter liquid, the homogeneous liquid is at 30 DEG C, when apparent viscosity is 45mpas, closes shear pump;
(5) homogeneous liquid is put into stirred tank, under stirring, is sequentially added into stirred tank spare
Lauric acid amide of ethanol, positive decyl glucoside, dimethyl silicone polymer, oleic acid base hydroxyethyl imidazole quinoline, isothiazolinone,
It is sufficiently stirred, stirring rate 190rpm, mixing time 30min;
(6) under stirring conditions, the uniform speed slow into stirred tank is pumped by circulation shear and paraffin oil, shear rate is added
For 170s-1, the shear agitation time is 2.0 hours, is obtained described without alveolitoid cleaning agent.
Embodiment 3
A kind of no alveolitoid cleaning agent of the present embodiment, the cleaning agent include lauric acid amide of ethanol 10kg, the positive last of the ten Heavenly stems
Base glucoside 15kg, dimethyl silicone polymer 1kg, oleic acid base hydroxyethyl imidazole quinoline 3kg, isothiazolinone 0.4kg, potassium acetate
11kg, xanthan gum 0.4kg, paraffin oil 55kg and water 40kg.
The preparation method without alveolitoid cleaning agent of the present embodiment, includes the following steps:
(1) it is weighed according to the weight of each component spare;
(2) weighed water is put into stirred tank, weighed potassium acetate is then added, stirs evenly, sufficiently dissolved, obtain
Acetic acid aqueous solutions of potassium is spare;
(3) under stirring conditions, weighed xanthan gum is added in acetic acid aqueous solutions of potassium, and heating stirring kettle, is added
Hot temperature is to 50 DEG C;
(4) solution that step (3) are heated is put into circulation shear kettle and is sheared, shear rate 200s-1, obtain
Matter liquid, the homogeneous liquid is at 30 DEG C, when apparent viscosity is 50mpas, closes shear pump;
(5) homogeneous liquid is put into stirred tank, under stirring, is sequentially added into stirred tank spare
Lauric acid amide of ethanol, positive decyl glucoside, dimethyl silicone polymer, oleic acid base hydroxyethyl imidazole quinoline, isothiazolinone,
It is sufficiently stirred, stirring rate 200rpm, mixing time 35min;
(6) under stirring conditions, the uniform speed slow into stirred tank is pumped by circulation shear and paraffin oil, shear rate is added
For 180s-1, the shear agitation time is 2.2 hours, is obtained described without alveolitoid cleaning agent.
Test example 1
Respectively to embodiment 1-3 preparation without alveolitoid cleaning agent carry out blistering rate, the condensate oil time, drain time, degree of corrosion,
Shale recovery ratio, flash-point, pour point are characterized, and the results are shown in Table 2, and measuring method is as follows.
1, blistering rate measuring method
The cleaning agent 400ml of embodiment 1-3 preparation is measured respectively in high-speed stirred cup, is existed by high frequency agitator
Under the conditions of 11000 ± 300 revs/min, high-speed stirred is after five minutes;Height a glass sample is stirred in 10 seconds to pour into 1000mL graduated cylinder, and
Volume is read in 10 seconds, is denoted as V;Blistering rate D is calculated with formula (1).
2, condensate oil time measuring method
In the cleaning solution 400ml high-speed stirred cup for measuring embodiment 1-3 preparation respectively, by high frequency agitator 11000
Under the conditions of ± 300 revs/min, high-speed stirred is after ten minutes;Height is stirred a glass sample to pour into 1000mL graduated cylinder, and starts timing, and
Time when it starts condensate oil is recorded, i.e., the oily time separated with water.
The present invention may determine that the stability of cleaning agent by the condensate oil time, and the condensate oil time, longer stability was better, condensate oil
Time is shorter, and stability is poorer.
3, drain time measuring method
3.1 standard test liquids are prepared
320ml 0# diesel oil is measured, 12.0g organoclay is added with stirring loading 11000 ± 300rpm, keeps stirring device,
16.0ml Span-80 is added with syringe, and quick lime 4.0g is added, high-speed stirred 10min.Machine is kept stirring, is slowly added to
80ml calcium chloride brine, the concentration of calcium chloride are 25%, add 24g sulfonated gilsonite, high-speed stirred 30min;Room temperature test is broken
Newborn voltage, it is desirable that emulsion-breaking voltage is greater than 400V;Increase Span-80 dosage if emulsion-breaking voltage is lower than 400V to it greater than 400V.
The preparation of 3.2 samples slurry
Three parts of 80ml clear water are measured respectively to be added in beaker, are added with stirring embodiment 1-3 loading 1000 ± 300rpm
The cleaning agent 4.0ml of preparation, keeps stirring device, continues to measure in the above-mentioned beaker of 20ml standard test liquid addition, stirs at low speed 1 point
Clock.
3.3 drain time
3.2 samples are poured into 100ml graduated cylinder, measuring its time that 20% clear water (16ml) is precipitated is drain time.
The present invention may determine that dissolution of the cleaning agent to oil base drilling fluid residue, dispersibility by drain time, and
It is found through experiments that and is able to satisfy the requirement of Oil Field application technology greater than 2min using showing that drain time is tested.
4, degree of corrosion measures
The preparation of 4.1 test steel discs
In dry conditions, No. 10 steel discs of 50mm × 25mm are chosen as test steel disc, the two sides of steel disc will be tested
And edge sand paper or emery cloth polishing it is bright;Portray a 40mm × 20mm's in No. 10 standard steel discs center of 50mm × 25mm
Box, and grid 50 of 4mm × 4mm are portrayed in box, grid line width is not more than 0.1mm.Test steel disc is immersed
In dehydrated alcohol, test steel disc is clamped with tweezers, is scrubbed with absorbent cotton, taken out and air-dry.
The evaluation of 4.2 degree of corrosion
By in 4.1 it is ready test steel disc immerse respectively embodiment 1-3 preparation without in alveolitoid greasy dirt detergent, be used in combination
Clear water does one group of parallel test, after being placed at room temperature for for 24 hours, takes out the corrosion situation on observation test steel disc surface, evaluation criterion is shown in Table
1。
Table 1
Corrode lattice number |
Degree of rusting (%) |
0 |
0 |
1-5 |
2-10 |
6-10 |
12-20 |
11-25 |
22-50 |
26-50 |
52-100 |
5, shale recovery ratio measures
The preparation of 5.1 test shale particles
By the shale particle broken into pieces by 5-10 the polished standard screen net, chooses shale particle of the partial size between 5-10 mesh and make
For test specimen.
5.2 shale recovery ratio evaluation experimentals
Respectively measure 300mL embodiment 1-3 preparation without alveolitoid greasy dirt detergent in high temperature ageing kettle, weigh 30g
It shale particle and is fallen in aging kettle in 5.1, is gently mixed uniformly with glass bar, obtains and test slurry;Slurry will be tested 100
After being rolled 16 hours under the conditions of DEG C, experiment slurry is taken out and passes through 100 mesh screens, then with clear water by sieve and shale particle
Surface washing is clean;Shale particle in 100 sieves is placed in thermostatic drying chamber, under the conditions of 105 ± 3 DEG C, freeze-day with constant temperature 4
After hour, taking-up is placed in drying basin after cooling 30 minutes, is weighed shale granular mass, is denoted as M;Shale is calculated with formula (2) to return
Yield:
6, flash(ing) test
Test sample open flash point is provided by GB/T 3536-2008.
7, pour point measurement
Test sample pour point is provided referring to GB/T 3535-2006.
Table 2
The above description is merely a specific embodiment, but scope of protection of the present invention is not limited thereto, any
Those familiar with the art in the technical scope disclosed by the present invention, can easily think of the change or the replacement, and should all contain
Lid is within protection scope of the present invention.Therefore, protection scope of the present invention should be based on the protection scope of the described claims.