CN105482787B - A kind of kneading process method that water-base drilling fluid fluid loss additive is prepared using anaerobic fermentation biogas residue - Google Patents
A kind of kneading process method that water-base drilling fluid fluid loss additive is prepared using anaerobic fermentation biogas residue Download PDFInfo
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Abstract
The present invention relates to a kind of oil field drilling fluids environmentally friendly fluid loss additive and its production and use, the raw material composition of the fluid loss additive includes：Natural polymer mixture biogas residue, basifier, organic solvent, etherifying agent, polysaccharide macromolecule dispersing agent, and crosslinking agent.Fluid loss additive prepared in accordance with the present invention has good heat and salinity tolerance ability, and cheap, production with it is environment-friendly during use, can be efficiently applied in fresh water, salt solution and compound salt-water drilling fluid system.
Description
Technical field
The invention belongs to the high level chemical utilization neck in oil field water-base drilling fluid inorganic agent field, and anaerobic fermentation biogas residue
Domain.More particularly to a kind of environmentally friendly heat and salinity tolerance fluid loss additive used in oil drilling and preparation method thereof and use
On the way.
Background technology
With the development of petroleum industry and the continuous growth of oil demand, oil-gas exploration and development is gradually to deep formation and sea
Upper development, the difficulty of drilling engineering is increasing, increasingly increased environmental pressure to environment-friendly type water base drilling fluid and drilling fluid at
The biodegradability of reason agent proposes requirements at the higher level.Water-base drilling fluid is by water, bentonite, inorganic and organic agent, rock
The complicated polymer suspension liquid system of the composition such as bits and some mineral materials, it is referred to as " blood " of drilling well, in oil/gas drilling work
Indispensable important function is played in journey.
One of the important process agent of fluid loss additive as water-base drilling fluid, play control filter loss, stabilizing borehole, in permeable formation
The effect such as thin tough fine and close mud cake is formed on diafiltration face, can effectively prevent the liquid in drilling fluid is percolated into stratum to cause ground
Layer swelling clay mineral, so that well collapses or injured oil and gas reservoir, to ensureing that safe, fast, efficient drilling well plays important work
With.
In additive for drilling fluid, fluid loss additive dosage is maximum, and species is various, predominantly natural material or natural material
Modified product and synthesized polymer species.Natural material or natural material modified product include humic acid, cellulose, lignin, shallow lake
Powder class and its derivative etc.；Synthetic polymer is mainly based on alkene monomer polymer class, synthetic resin etc., but by monomer kind
Class is more, polymer architecture is complicated, relative molecular mass is changeable, the limitation of price very high condition, such synthetic polymer scene
Using less.The more fluid loss additive of commercial Application is mainly all kinds of modified natural polymer materials.
Natural material is cheap and easy to get as fluid loss additive, but the structure due to natural material and group limitation, temperature resistance,
It can not meet needs in terms of anti-salt property.Using the active group enriched in natural products, reacted, be grafted by polymer chemistry
The processing such as copolymerization, while material script performance is kept, improves the heat and salinity tolerance ability of product, makes it in oil drilling
It is widely applied.It is superior by the modified general heat-resisting property of humic-acid kind fluid loss additive, but salt-resistance is poor；It is modified to form sediment
Powder class and cellulose family fluid loss additive, heatproof have good salt tolerance up to 120 DEG C or so, available for saturated brine with
In seawater, but the major defect of modified starch is that biological stability is poor, and the biological stability of modified cellulose compares modified starch
It is a little better；Modified lignin resin is typically reacted with formaldehyde, phenol, urea, vinyl monomer etc. one to prepare resinae drop
Fluid loss agents, because it contains substantial amounts of hydrophilic radical, there is the performances such as good heatproof, salt tolerant, resistance to calcium ions and magnesium ions, but make
In, there is serious bubble problem in such modified resin, coordinate defoamer to use.
Molecular modification is carried out to natural products molecule, by changing the means such as group, side-chain structure, is keeping natural products
On the premise of environment-friendly, it is expected to obtain high performance-price ratio fluid loss additive product, brainstrust has carried out numerous studies work in this respect
Make.Such as：
Chinese patent CN101255333A is proposed by introducing quaternary ammonium cation and crosslinking agent in the reaction so that it forms sediment
The advantages of compound powder is reached with cationic starch, crosslinked starch and gelatinized starch, has a good temperature resistance, but for
Salt-resistance does not refer to but.The utilization existing process that Chinese patent CN101602938A is proposed prepares cellulose base drop with equipment and filtered
The method for losing agent, can not still solve the problems such as big organic solvent usage amount, product post processing.Chinese patent CN103396515A
It is raw material to propose using starch, phenolic compound, eneamide, olefin sulfonic acid, and oil-phase solution is continuous phase, emulsifying agent,
Reduce under substrate and hydrogen acceptor substrate catalytic action, prepare a kind of starch graft copolymer fluid loss additive, there is good resist
Temperature, salt resistance, anticalcium ability, but requirement of this method to raw material is more strict, and course of reaction is complicated, and a large amount of alkenes introduce, no
Beneficial to biodegradation.
By drilling cost control constraints, drilling contractor requires constantly to reduce the cost of additive for drilling fluid.Therefore, have perhaps
More researchers have developed with maize straw, bagasse, soybean residue, fecula, furfural from cheap alternative materials are found
Slag, former short velveteen etc. are the carboxymethyl cellulose derivative of raw material.But these industrial or agricultural by-product raw material will often first pass through
Complicated pretreatment could be used to produce, and the temperature resistance of its product carboxymethyl cellulose derivative and salt-resistance are often up to not
The LV-CMC (low viscous sodium carboxymethylcellulose) or CMS (CMS) use quality standard commonly used to oil drilling industry
It is required that, it is difficult to it is substituted completely is used as the environment-friendly type fluid loss additive of water-base drilling fluid.As United States Patent (USP) US7384892B2 is proposed
Prepare fluid loss additive CM-RCL using former short velveteen, can be modified afterwards by non-ionic group or ionic group processing with
Other excellent properties are obtained, salt-resistance, increase viscosity, regulation yield value and gel strength is such as improved, achieves preferably
Effect, but need to crush former short velveteen in inert gas and to retain original cellulosic polymer feature knot
Structure, along with short velveteen price more and more higher, cause the cost more and more higher of this method.Chinese patent CN101768220A is proposed
It is a kind of using landing method of the cotton for carboxymethyl cellulose, by cellulose activation, afterwards be etherified, neutralize, washing
Process carries out carboxy methylation, and this method has widened the raw material of production carboxymethyl cellulose, but needs are purified to landing cotton, essence
System etc..Chinese patent CN103861570A proposes a kind of new bagasse sorbing material and preparation method thereof, wherein select
Sugarcane obtains bagasse powder, recycles proteases for decomposing bagasse through over cleaning, peeling, broken, drying, crushing, sieving etc.
In unnecessary protein, use alkaline reaction again afterwards, neutralized with watery hydrochloric acid, can be utilized after drying, in a word pretreatment condition
It is very complicated, it have impact on its high-valued utilization.《Fine chemistry industry》Magazine 1996 year the 3rd phase of volume 13 has delivered Yanan University Yang De
Congruence has produced the carboxymethyl potato slag product that substitution value reaches 0.8 on the carboxymethylated technical study of potato residues；
《Agriculture of Anhui science》The magazine 2010 year phase of volume 38 33 has delivered Lanzhou University Bai Zhonglan etc. and has prepared carboxylic on potato starchy residue
The research of methylcellulose and CMS mixture, the substitution value of product need to remove in raw material in advance up to 0.5
The impurity such as lignin, hemicellulose, fat, a small amount of albumen, add reaction cost and practical operation difficulty, limit it and apply valency
Value.
With the fast development of biomass energy, the residue biogas residue resource after large-sized biogas engineering anaerobic fermentation is also more next
It is abundanter, presently mainly used as organic compost, feed addictive etc., its added value is relatively low, and exist and pollute, waste,
Security problems, the problems such as local soil eutrophication, water pollution are caused when making organic compost such as biogas residue, making feed addition
Contain antibiotic agents during agent for it and its still need to further study the problem of influenceing human and livestock health.
Study discovery with keen determination by the present inventor, grain base grain slag is most by caused biogas residue after anaerobic fermentation
Carbohydrate is depleted, and a part of residual lignin, cellulose, hemicellulose have been in alienation state, and microbial action makes natural pond
Slag little particle is in serious irregular shape, and structure combines more open between each other, and crystallinity reduces a lot, surface and internal production
Substantial amounts of cavity and crack have been given birth to, has been advantageous to infiltration of the chemical reagent to its inside configuration, substantially increases chemical reactivity,
It is especially suitable for doing the raw material to chemically react.Such advantage allows it to be separated without component, directly with biogas residue natural polymer
Sub- mixture is that raw material is handled via different physics-chemical technology, and deep processing is the high property with higher heat and salinity tolerance ability
Valency also can be that biomass biogas residue creates higher warp while solving the problems, such as component environment than natural polymer fluid loss additive
Ji benefit.
Table 1 is the main chemical compositions of residue of the Moutai (Spirit) factory spirit stillage after anaerobic ferment for methane, can
To find out, as the biogas residue of natural polymer mixture, its main component is not and the fully residual lignin of anaerobic fermentation, fibre
Tie up the materials such as element, hemicellulose.
Table 1：A kind of main constituents (wt%) of spirit stillage anaerobic fermentation biogas residue
| Detection project | Detection one | Detection two | Detection three | Average value |
| Thick slag total organic matter | 84.10 | 83.26 | 82.84 | 83.40 |
| Fine slag total organic matter | 68.92 | 68.89 | 68.91 | 68.91 |
| Thick slag lignin | 27.66 | 29.78 | 28.72 | 28.72 |
| Thick slag cellulose | 28.42 | 25.50 | 26.96 | 26.96 |
| Thick slag hemicellulose | 17.22 | 18.34 | 17.88 | 17.81 |
| Fine slag lignin | 13.28 | 13.30 | 13.29 | 13.29 |
| Fine slag cellulose | 4.33 | 4.32 | 4.34 | 4.33 |
| Fine slag hemicellulose | 9.82 | 9.80 | 9.84 | 9.82 |
The content of the invention
In being actually used for existing natural polymer fluid loss additive the defects of the heat and salinity tolerance scarce capacity of generally existing,
The problem to be solved in the present invention is to find cheap raw material, and then develops a kind of suitable preparation method to synthesize a kind of environment
The heat and salinity tolerance fluid loss additive of friendly, the fluid loss additive should have that environment-friendly, filtrate loss controllability is superior, there have to be certain anti-
Warm saline-alkaline tolerance, lower-price characteristic, performance reach LV-CMC standard, better than CMS, applied to fresh water, salt solution and compound
In DWSW liquid system.
Therefore, the present invention is realized by such technology path：For cellulose, half fibre mainly contained in biogas residue
Dimension element, lignin progress are etherification modified, and being formed has certain water miscible flocculation mixture；Polysaccharide dispersant
It is blended in biogas residue raw material, it is possible to increase the contact area between reaction reagent, improve etherification reaction degree；Crosslinking agent will naturally change
Property macromolecule mixture and polysaccharide dispersant carry out cross-linking reaction, form certain space net structure, and then improve this hair
The heat and salinity tolerance ability of publicly price-reduction fluid loss agents, it is set to be applied in fresh water, salt solution, compound salt solution and deep-well complex drilling liquid system.
By the research with keen determination of the present inventor, invent and provide a kind of Environment-protecting Drilling Fluids fluid loss additive, it is by price
Cheap combination of raw materials is made, and specifically, its raw material composition includes：Natural polymer biogas residue, basifier, organic solvent,
Etherifying agent, polysaccharide macromolecule dispersing agent, and crosslinking agent.
Wherein each raw material composition and respective quality proportioning are：
Natural polymer (or its mixture) biogas residue, 8~30 parts, preferably 10~25 parts, more preferably 15~25 parts,
Basifier, 5~20 parts, preferably 8~16 parts, more preferably 10~16 parts,
Organic solvent, 10~80 parts, preferably 20~60 parts, more preferably 30~50 parts,
Etherifying agent, 5~20 parts, preferably 8~16 parts, more preferably 10~16 parts,
Polysaccharide macromolecule dispersing agent, 1~10 part, preferably 3~8 parts, more preferably 5~8 parts,
Crosslinking agent, 0.5~8 part, preferably 1~5 part, more preferably 2~4 parts,
The above-mentioned further feature of these components that the present inventor is previously mentioned includes：
The natural polymer mixture biogas residue is the residue after grain base grain slag anaerobic fermentation,
The basifier is the strong basicity inorganic reagents such as sodium hydroxide, potassium hydroxide,
The organic solvent is the mixed solvent of water and small molecule alcohol, and the organic solvent is preferably water and methanol, second
Alcohol, propyl alcohol, isopropanol, ethylene glycol, butanol etc. be one or two kinds of or the mixed solvent of two or more compositions, quality shared by its reclaimed water
Percentage is 10%~75%, but when convenience security of synthesis technique etc. considers from sexual valence, the small molecule alcohol
Preferred alcohol and isopropanol,
Organic etherifying agent is used for chemical modification, is one or both of monoxone, sodium chloroacetate etc.
The polysaccharide macromolecule dispersing agent improves etherification reaction degree, be modified starch derivative one or two or
The mixture of two or more compositions,
The crosslinking agent makes polymer form network structure, is water-soluble silicate class, silane coupler, formaldehyde, epoxy
The mixture of one or both of chloropropane etc. or two or more compositions, but from obtained crosslinked polymeric salt-resistance
Consider, preferably water-soluble silicate.
By the research with keen determination of the present inventor, also further invent and provide a kind of preparation side of environment-friendly type fluid loss additive
Method.Its each raw material composition and its quality proportioning are：
Natural polymer (or its mixture) biogas residue, 8~30 parts, preferably 10~25 parts, more preferably 15~25 parts,
Basifier, 5~20 parts, preferably 8~16 parts, more preferably 10~16 parts,
Organic solvent, 10~80 parts, preferably 20~60 parts, more preferably 30~50 parts,
Etherifying agent, 5~20 parts, preferably 8~16 parts, more preferably 10~16 parts,
Polysaccharide macromolecule dispersing agent, 1~10 part, preferably 3~8 parts, more preferably 5~8 parts,
Crosslinking agent, 0.5~8 part, preferably 1~5 part, more preferably 2~4 parts,
The preparation method comprises the following steps：
1) pretreatment of biogas residue：Biogas residue raw material are subjected to primary dcreening operation, crushing and/or sieving,
2) pretreated biogas residue and dispersant are weighed, crushes and mixes,
3) basifier and crosslinking agent are weighed, is dissolved in the water for preparing organic solvent, is added after uniformly cooling to be dissolved small
Molecule alcohols, obtains solution,
4) solid powder that step 2) obtains is added in the solution that step 3) obtains, and stirring, is mediated uniformly, and carry out alkali
Change reaction,
5) alkalization is finished after adding etherifying agent in the mixture that step 4) obtains, and is heated up and is carried out etherification reaction,
6) mixture that step 5) is obtained after being etherified is dried and/or crushed.
Specific technology of preparing scheme is as described below：
1) pretreatment of biogas residue：Biogas residue raw material are subjected to primary dcreening operation, the debris such as the sandstone of the inside is removed, crushes afterwards, mistake
50~100 mesh, preferably 55~80 mesh, more preferably 60 the polished standard screens, it is standby,
2) the pretreated biogas residue of said ratio and dispersant are weighed, is crushed, is well mixed, it is standby,
3) basifier and crosslinking agent of said ratio are weighed, is dissolved in the water for preparing organic solvent, it is to be dissolved uniformly cold
But the small molecule alcohol of said ratio is added afterwards, obtains homogeneous solution
4) solid powder that step 2) obtains is added in the solution that step 3) obtains, stirring, is mediated uniformly, 10~60
DEG C, several minutes of quaternization is carried out under the conditions of preferably 15~45 DEG C, more preferably 25~30 DEG C to a few hours, preferably 30min to 3h,
More preferably 45min to 2h, such as 60min,
5) alkalization is finished after adding etherifying agent in the mixture that step 4) obtains, and is warming up to 60~95 DEG C, preferably 70~
85 DEG C, more preferably 80~85 DEG C carry out several minutes of etherification reaction to a few hours, preferably 30min to 3h, more preferably 45min to 2h,
Such as 60min,
6) mixture that step 5) is obtained after being etherified is placed in 70~120 DEG C, preferably 85~110 DEG C, more preferably 105
At~110 DEG C, dry, crush.
Dropped and filtered with environment-friendly type natural polymer by the foregoing oil field drilling fluids obtained by the above method of the present invention
Aquation clay systems space structure can be controlled by losing agent, obtain the filtrate loss controllability of preferable heat and salinity tolerance.
Therefore, natural polymer fluid loss additive LV-CMC and CMS existing compared in the market etc., oil drilling of the invention
Liquid environment-friendly type natural polymer fluid loss additive has advantages below：
1st, raw material sources are extensive, and cost is more cheap；
2nd, higher value application is carried out to biogas residue, and it is transformed into the product with certain added value, it is both economically and environmentally beneficial；
3rd, product has preferable heat and salinity tolerance filtrate loss controllability, and wherein normal temperature fresh water filtrate reducing rate is more than 90%, always
(120 DEG C of aging 16h) fresh water filtrate reducing rate is more than 90% after change, and normal temperature saturated brine filtrate reducing rate is more than 90%, aging
(120 DEG C of aging 16h) saturated brine filtrate reducing rate is more than 85% afterwards.
Brief description of the drawings
Fig. 1 is the environmentally friendly fluid loss additive preparation technology flow chart of the present invention.
Embodiment
It is further explained and described present invention by the following examples.But the embodiment provided is not understood that
To be construed as limiting to the scope of the present invention.
Performance evaluation
1. sample appearance is evaluated
Sample is estimated at normal temperatures
2. moisture is evaluated
Water content is sample the ratio between quality of reduction and sample mass after 105 ± 3 DEG C of drying constant weights, with percentage table
Show.5g samples (claiming accurate to 0.0001g) are weighed, is placed in the measuring cup of known quality, is dried 2h in 105 ± 3 DEG C, be placed in drying
Room temperature is cooled in device, weighs and (claims accurate to 0.0001g).Moisture is calculated by formula 1.
In formula：W-water content, %；
m1- measuring cup quality, g；
m2Measuring cup and sample mass, g before-drying；
m3Measuring cup and sample mass, g after-drying.
3.pH values determine
Weigh and (claim accurate to 0.01g) in 105 ± 3 DEG C of sample 1g for drying 2h, addition 2mL ethanol wets, which are placed in, to be filled
In the beaker of 100mL distilled water, stirred with electric mixer to complete molten, its pH value is determined with acidometer or accurate pH test paper.
4. filtrate loss controllability is evaluated
(1) preparation of base slurry
The preparation of fresh water-based slurry：Soil, 2.80gNaHCO are evaluated by 100.00g Britain is added in 1000.00mL distilled water3's
Ratio prepares base slurry, high-speed stirred 20min, at least stops therebetween twice, to scrape the clay of adhesion on the wall.25 ±
Curing in airtight condition 24h at 3 DEG C.The API filtration of the fresh water-based slurry prepared should be in 50~60mL/30min.
The preparation of saturation NaCl brine muds：By added in 1000.00mL distilled water 100.00g Britain evaluation soil,
365.00gNaCl、2.80gNaHCO3Ratio prepare base slurry, high-speed stirred 20min, at least stop therebetween twice, it is viscous to scrape
Attached clay on the wall.The curing in airtight condition 24h at 25 ± 3 DEG C.The API filtration of the water base slurry of saturation prepared should be
100~110mL/30min.
(2) measure of API filtration
The slurry of the base after 400.00mL curing in airtight condition is measured, 6.00g samples is added, filtration device is poured into after high-speed stirred 20min
To at graduation mark in cup, first plus good sealing ring is then placed in filter paper, covers cup lid.Graduated cylinder is placed on filter press filtrate (liquid
Under, 0.69MPa is forced into, opens intake valve timing simultaneously.The volume for the filtrate that 30min is collected is recorded, is designated as the brill before aging
Well liquid filter loss (i.e. API filtration).
(3) heat-resisting property determines
The slurry of the base after 400.00mL curing in airtight condition is measured, 6.00g samples is added, ageing can is poured into after high-speed stirred 20min
In, roller heating stove is put into, constant temperature rolls at 120 DEG C, aging 16h.Take out ageing can be slowly cooled to room temperature, pour out, it is high
Speed stirring 5min, the drilling fluid filtration (i.e. API filtration) after aging is carried out according to the method in (2) and is tested.
Embodiment raw materials
Residue of Moutai (Spirit) factory of the biogas residue system spirit stillage after anaerobic ferment for methane.
Polysaccharide family macromolecule dispersing aid SYM, SHS, STD, SMS are industrial goods, are to have purchased from the grand industry and trade of Beijing Hong Chang
Limit the series modified starch derivatives of responsible company.
Etherifying agent system purchases the technical grade monoxone (MCA) from Yancheng City prize chemical industry Co., Ltd of Jiangsu Province.
Crosslinking agent system purchases the technical grade solid sodium metasilicate (mould from Red Star spacious mansion chemical building material Co., Ltd of Beijing
Number 3.0).
Caustic soda (NaOH), ethanol (CH3CH2OH), epoxychloropropane (C3H5) etc. ClO chemical reagent is the pure level of analysis
(AR) it is, to purchase from Beijing Chemical Plant.
Embodiment
Embodiment 1：
Weigh alkaline agent sodium hydroxide 18.50g and cross-linking agent sodium 4.00g is dissolved in 30.00mL water, it is to be dissolved uniform
30.00mL ethanol is added after cooling, is configured to homogeneous solution, the reaction solution as prepared；By pretreated biogas residue
22.50g and dispersing aid SHS 7.50g is crushed, is well mixed, is added in reaction solution, after being uniformly mixed, at 25 DEG C
Mediate alkalization 60min；Etherifying agent monoxone 18.50g is added after alkalization, is stirred, is mediated, the etherification reaction at 85 DEG C
60min；Obtained mixture is placed at 85 DEG C, dried, crushes, produces sample.Embodiment 1 is commented according to above fluid loss additive
Price card standard is tested, and detection data are shown in Table 2.
Table 2：The quality measurements of embodiment 1
Embodiment 2：
It is with the difference of embodiment 1：Dispersing aid adds species.Weigh alkaline agent sodium hydroxide 18.50g and crosslinking agent silicic acid
Sodium 4.00g is dissolved in 30.00mL water, is added 30.00mL ethanol after uniformly cooling to be dissolved, is configured to homogeneous solution, i.e.,
For the reaction solution of preparation；Pretreated biogas residue 22.50g and dispersing aid SYM 7.50g is crushed, be well mixed, is added to
In reaction solution, after being uniformly mixed, alkalization 60min is mediated at 25 DEG C；Etherifying agent monoxone is added after alkalization
18.50g, stir, mediate, the etherification reaction 60min at 85 DEG C；Obtained mixture is placed at 85 DEG C, dried, powder
It is broken, produce sample.Embodiment 2 is tested according to above fluid loss additive evaluation criterion, detection data are shown in Table 3.
Table 3：The quality measurements of embodiment 2
Embodiment 3：
It is with the difference of embodiment 1：Dispersing aid adds species.Weigh alkaline agent sodium hydroxide 18.50g and crosslinking agent silicic acid
Sodium 4.00g is dissolved in 30.00mL water, is added 30.00mL ethanol after uniformly cooling to be dissolved, is configured to homogeneous solution, i.e.,
For the reaction solution of preparation；Pretreated biogas residue 22.50g and dispersing aid STD 7.50g is crushed, be well mixed, is added to
In reaction solution, after being uniformly mixed, alkalization 60min is mediated at 25 DEG C；Etherifying agent monoxone is added after alkalization
18.50g, stir, mediate, the etherification reaction 60min at 85 DEG C；Obtained mixture is placed at 85 DEG C, dried, powder
It is broken, obtain sample.Embodiment 3 is tested according to above fluid loss additive evaluation criterion, detection data are shown in Table 4.
Table 4：The quality measurements of embodiment 3
Embodiment 4:
It is with the difference of embodiment 1：Dispersing aid adds species.Weigh alkaline agent sodium hydroxide 18.50g and crosslinking agent silicic acid
Sodium 4.00g is dissolved in 30.00mL water, is added 30.00mL ethanol after uniformly cooling to be dissolved, is configured to homogeneous solution, i.e.,
For the reaction solution of preparation；Pretreated biogas residue 22.50g and dispersing aid SMS 7.50g is crushed, be well mixed, is added to
In reaction solution, after being uniformly mixed, alkalization 60min is mediated at 25 DEG C；Etherifying agent monoxone is added after alkalization
18.50g, stir, mediate, the etherification reaction 60min at 85 DEG C；Obtained mixture is placed at 85 DEG C, dried, powder
It is broken, produce sample.Embodiment 4 is tested according to above fluid loss additive evaluation criterion, detection data are shown in Table 5.
Table 5：The quality measurements of embodiment 4
Embodiment 5:
It is with the difference of embodiment 3：Crosslinking agent addition is reduced.Weigh alkaline agent sodium hydroxide 18.50g and crosslinking agent silicic acid
Sodium 3.00g is dissolved in 30.00mL water, is added 30.00mL ethanol after uniformly cooling to be dissolved, is configured to homogeneous solution, i.e.,
For the reaction solution of preparation；Pretreated biogas residue 22.50g and dispersing aid STD 7.50g is crushed, be well mixed, is added to
In reaction solution, after being uniformly mixed, alkalization 60min is mediated at 25 DEG C；Etherifying agent monoxone is added after alkalization
18.50g, stir, mediate, the etherification reaction 60min at 85 DEG C；Obtained mixture is placed at 85 DEG C, dried, powder
It is broken, obtain sample.Embodiment 5 is tested according to above fluid loss additive evaluation criterion, detection data are shown in Table 6.
Table 6：The quality measurements of embodiment 5
Embodiment 6:
It is with the difference of embodiment 3：The increase of crosslinking agent addition.Weigh alkaline agent sodium hydroxide 18.50g and crosslinking agent silicic acid
Sodium 5.00g is dissolved in 30.00mL water, is added 30.00mL ethanol after uniformly cooling to be dissolved, is configured to homogeneous solution, i.e.,
For the reaction solution of preparation；Pretreated biogas residue 22.50g and dispersing aid STD 7.50g is crushed, be well mixed, is added to
In reaction solution, after being uniformly mixed, alkalization 60min is mediated at 25 DEG C；Etherifying agent monoxone is added after alkalization
18.50g, stir, mediate, the etherification reaction 60min at 85 DEG C；Obtained mixture is placed at 85 DEG C, dried, powder
It is broken, obtain sample.Embodiment 6 is tested according to above fluid loss additive evaluation criterion, detection data are shown in Table 7.
Table 7：The quality measurements of embodiment 6
Embodiment 7
It is with the difference of embodiment 3：Crosslinking agent adds species.Weigh alkaline agent sodium hydroxide 18.50g and crosslinking agent epoxy chlorine
Propane 4.00g is dissolved in 30.00mL water, is added 30.00mL ethanol after uniformly cooling to be dissolved, is configured to homogeneous solution,
The reaction solution as prepared；Pretreated biogas residue 22.50g and dispersing aid STD 7.50g is crushed, be well mixed, is added
Into reaction solution, after being uniformly mixed, alkalization 60min is mediated at 25 DEG C；Etherifying agent monoxone is added after alkalization
18.50g, stir, mediate, the etherification reaction 60min at 85 DEG C；Obtained mixture is placed at 85 DEG C, dried, powder
It is broken, produce sample.Embodiment 7 is tested according to above fluid loss additive evaluation criterion, detection data are shown in Table 8.
Table 8：The quality measurements of embodiment 7
Embodiment 8
It is with the difference of embodiment 3：Change pretreatment biogas residue and the addition of dispersant.Weigh alkaline agent sodium hydroxide
18.50g and cross-linking agent sodium 4.00g are dissolved in 30.00mL water, are added 30.00mL ethanol after uniformly cooling to be dissolved, are matched somebody with somebody
Homogeneous solution is made, the reaction solution as prepared；By pretreated biogas residue 15.00g and dispersing aid STD15.00g powder
It is broken, well mixed, it is added in reaction solution, after being uniformly mixed, alkalization 60min is mediated at 25 DEG C；Add after alkalization
Enter etherifying agent monoxone 18.50g, stir, mediate, the etherification reaction 60min at 85 DEG C；Obtained mixture is placed in 85
At DEG C, dry, crush, produce sample.Embodiment 8 is tested according to above fluid loss additive evaluation criterion, detection data are shown in
Table 9.
Table 9：The quality measurements of embodiment 8
Embodiment 9
It is with the difference of embodiment 3：Change pretreatment biogas residue and the addition of dispersing aid.Weigh alkaline agent sodium hydroxide
18.50g and cross-linking agent sodium 4.00g are dissolved in 30.00mL water, are added 30.00mL ethanol after uniformly cooling to be dissolved, are matched somebody with somebody
Homogeneous solution is made, the reaction solution as prepared；By pretreated biogas residue 10.00g and dispersing aid STD20.00g powder
It is broken, well mixed, it is added in reaction solution, after being uniformly mixed, alkalization 60min is mediated at 25 DEG C；Add after alkalization
Enter etherifying agent monoxone 18.50g, stir, mediate, the etherification reaction 60min at 85 DEG C；Obtained mixture is placed in 85
At DEG C, dry, crush, produce sample.Embodiment 9 is tested according to above fluid loss additive evaluation criterion, detection data are shown in
Table 10.
Table 10：The quality measurements of embodiment 9
Comparative example 1
The sample that embodiment 3 the is prepared oil field fluid loss additive more ripe with field application in the market
LV-CMC, CMS CMS test according to above fluid loss additive Performance evaluation criterion, and detection data are shown in Table 11.
Table 11：The quality measurements of comparative example 1
Contrasted from above-described embodiment 1-9 and comparative example 1 filtrate loss controllability, comparing result is shown in Table 12.
Table 12：The filtrate loss controllability of the embodiment of the present invention and its contrast with LV-CMC, CMS
As can be seen from Table 12, the environmentally friendly fluid loss additive performance prepared by the present invention is generally preferable, its product
Performance is also suitable with LV-CMC with oil field, is superior to CMS CMS, can substitute it completely applied to fresh water, salt solution, compound
In salt solution and complex drilling liquid system.
The present invention is described in detail according to the above embodiments.It should be noted that the embodiment of the above just to
Illustrate the present invention.On the premise of without departing from spirit and substance of the present invention, those skilled in the art can design
Go out a variety of alternatives and improvement project of the present invention, it all should be interpreted within protection scope of the present invention.
Claims (10)
1. a kind of preparation method of filtrate reducer for oil field well drilling fluid, the raw material composition of the filtrate reducer for oil field well drilling fluid and
Respective quality proportioning is：
Natural polymer mixture biogas residue, 8~30 parts,
Basifier, 5~20 parts,
Organic solvent, 10~80 parts,
Etherifying agent, 5~20 parts,
Polysaccharide macromolecule dispersing agent, 1~10 part,
Crosslinking agent, 0.5~8 part,
The preparation method comprises the following steps：
1) pretreatment of biogas residue：Biogas residue raw material are subjected to primary dcreening operation, crushing and/or sieving,
2) pretreated biogas residue and dispersant are weighed, crushes and mixes,
3) basifier and crosslinking agent are weighed, is dissolved in the water for preparing organic solvent, small molecule is added after uniformly cooling to be dissolved
Alcohols, solution is obtained,
4) solid powder that step 2) obtains is added in the solution that step 3) obtains, and stirring, is mediated uniformly, and alkalize instead
Should,
5) alkalization is finished after adding etherifying agent in the mixture that step 4) obtains, and is heated up and is carried out etherification reaction,
6) mixture that step 5) is obtained after being etherified is dried and/or crushed.
2. preparation method according to claim 1, it is characterised in that the raw material group of the filtrate reducer for oil field well drilling fluid
Into and respective quality proportioning be：
Natural polymer mixture biogas residue, 10~25 parts,
Basifier, 8~16 parts,
Organic solvent, 20~60 parts,
Etherifying agent, 8~16 parts,
Polysaccharide macromolecule dispersing agent, 3~8 parts,
Crosslinking agent, 1~5 part.
3. preparation method according to claim 2, the raw material composition of the filtrate reducer for oil field well drilling fluid and respective
Quality proportioning is：
Natural polymer mixture biogas residue, 15~25 parts,
Basifier, 10~16 parts,
Organic solvent, 30~50 parts,
Etherifying agent, 10~16 parts,
Polysaccharide macromolecule dispersing agent, 5~8 parts,
Crosslinking agent, 2~4 parts.
4. the preparation method according to one of claims 1 to 3, it is characterised in that：
The natural polymer mixture biogas residue is the residue after grain base grain slag anaerobic fermentation, and/or
The basifier is sodium hydroxide, potassium hydroxide, and/or
The organic solvent is the mixed solvent of water and small molecule alcohol, and/or
Organic etherifying agent is used for chemical modification, is monoxone, one or both of sodium chloroacetate, and/or
The polysaccharide macromolecule dispersing agent improves etherification reaction degree, for the one or two of modified starch derivative or two kinds
The mixture of composition described above, and/or
The crosslinking agent makes polymer form network structure, is water-soluble silicate class, silane coupler, formaldehyde, epoxy chloropropionate
The mixture of one or both of alkane or two or more compositions.
5. preparation method according to claim 4, it is characterised in that the organic solvent is water and methanol, ethanol, third
The mixed solvent of one or both of alcohol, isopropanol, ethylene glycol, butanol or two or more compositions, quality hundred shared by its reclaimed water
Divide than being 10%~75%.
6. preparation method according to claim 4, it is characterised in that the small molecule alcohol is ethanol and isopropanol.
7. preparation method according to claim 1, comprises the following steps：
1) pretreatment of biogas residue：Biogas residue raw material are subjected to primary dcreening operation, the sandstone debris of the inside is removed, crushes afterwards, cross 50~100
The polished standard screen, it is standby,
2) pretreated biogas residue and dispersant are weighed by proportioning, crushed, is well mixed, it is standby,
3) basifier and crosslinking agent are weighed by proportioning, be dissolved in the water for preparing organic solvent, added after uniformly cooling to be dissolved
Small molecule alcohol, homogeneous solution is obtained,
4) solid powder that step 2) obtains is added in the solution that step 3) obtains, stirring, mediates uniform, 10~60 DEG C of conditions
Lower several minutes of quaternization of progress to a few hours,
5) alkalization is finished after adding etherifying agent in the mixture that step 4) obtains, and is warming up to 60~95 DEG C of progress etherification reaction numbers
Minute to a few hours,
6) mixture that step 5) is obtained after being etherified is placed at 70~120 DEG C, is dried, and is crushed.
8. preparation method according to claim 7, it is characterised in that
Step 3)~4) in reaction temperature persistently control at 25~30 DEG C, and/or,
Step 5) reaction temperature is controlled at 80~85 DEG C, and/or,
Step 6) drying temperature is controlled at 105~110 DEG C.
9. filtrate reducer for oil field well drilling fluid made from the method according to one of claim 1 to 8, it is environment-friendly type drilling well
Liquid fluid loss additive, wherein normal temperature fresh water filtrate reducing rate is more than 90%, and fresh water filtrate reducing rate is 90% after 120 DEG C of aging 16h
More than；Normal temperature saturated brine filtrate reducing rate is more than 90%, and the saturated brine filtrate reducing rate after 120 DEG C of aging 16h is 85%
More than.
10. the purposes of fluid loss additive according to claim 9, it can be controlled as filtrate reducer for oil field well drilling fluid
Aquation clay systems space structure, obtain the filtrate loss controllability of preferable heat and salinity tolerance.
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| CN101003577A (en) * | 2006-01-20 | 2007-07-25 | 上海长光企业发展有限公司 | Technique for producing polyanionic cellulose with high degree of substitution |
| CN101033257A (en) * | 2007-03-09 | 2007-09-12 | 北京理工大学 | Method of preparing high substitution degree low viscosity polyanionic cellulose |
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| CN101003577A (en) * | 2006-01-20 | 2007-07-25 | 上海长光企业发展有限公司 | Technique for producing polyanionic cellulose with high degree of substitution |
| CN101033257A (en) * | 2007-03-09 | 2007-09-12 | 北京理工大学 | Method of preparing high substitution degree low viscosity polyanionic cellulose |
| CN101838334A (en) * | 2009-03-19 | 2010-09-22 | 上海长光企业发展有限公司 | Preparation method of high viscosity polyanion cellulose |
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