CN105860943A - Inhibited type starch filtrate reducer for drilling fluid and preparation method of inhibited type starch filtrate reducer - Google Patents
Inhibited type starch filtrate reducer for drilling fluid and preparation method of inhibited type starch filtrate reducer Download PDFInfo
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- CN105860943A CN105860943A CN201610256544.3A CN201610256544A CN105860943A CN 105860943 A CN105860943 A CN 105860943A CN 201610256544 A CN201610256544 A CN 201610256544A CN 105860943 A CN105860943 A CN 105860943A
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- Prior art keywords
- starch
- polymine
- drilling fluid
- suppressive
- loss additive
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K8/00—Compositions for drilling of boreholes or wells; Compositions for treating boreholes or wells, e.g. for completion or for remedial operations
- C09K8/02—Well-drilling compositions
- C09K8/04—Aqueous well-drilling compositions
- C09K8/14—Clay-containing compositions
- C09K8/18—Clay-containing compositions characterised by the organic compounds
- C09K8/20—Natural organic compounds or derivatives thereof, e.g. polysaccharides or lignin derivatives
- C09K8/206—Derivatives of other natural products, e.g. cellulose, starch, sugars
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B31/00—Preparation of derivatives of starch
- C08B31/08—Ethers
- C08B31/12—Ethers having alkyl or cycloalkyl radicals substituted by heteroatoms, e.g. hydroxyalkyl or carboxyalkyl starch
- C08B31/125—Ethers having alkyl or cycloalkyl radicals substituted by heteroatoms, e.g. hydroxyalkyl or carboxyalkyl starch having a substituent containing at least one nitrogen atom, e.g. cationic starch
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G81/00—Macromolecular compounds obtained by interreacting polymers in the absence of monomers, e.g. block polymers
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K8/00—Compositions for drilling of boreholes or wells; Compositions for treating boreholes or wells, e.g. for completion or for remedial operations
- C09K8/02—Well-drilling compositions
- C09K8/04—Aqueous well-drilling compositions
- C09K8/14—Clay-containing compositions
- C09K8/18—Clay-containing compositions characterised by the organic compounds
- C09K8/22—Synthetic organic compounds
- C09K8/24—Polymers
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Materials Engineering (AREA)
- Engineering & Computer Science (AREA)
- Life Sciences & Earth Sciences (AREA)
- Medicinal Chemistry (AREA)
- Dispersion Chemistry (AREA)
- Polymers & Plastics (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Biochemistry (AREA)
- Polysaccharides And Polysaccharide Derivatives (AREA)
Abstract
The invention relates to an inhibited type starch filtrate reducer for a drilling fluid and a preparation method of the inhibited type starch filtrate reducer. The inhibited type starch filtrate reducer for the drilling fluid is prepared from the following main raw materials of starch, a bridging agent and a poly-amido compound through etherification reaction in deionized water under the action of a catalyst. The inhibited type starch filtrate reducer for the drilling fluid is prepared by the starch, the bridging agent and the polyamine compound through etherification reaction, and a starch molecular chain in a product is rich in amido group, and can generate a multi-point adsorption effect with stratum clay minerals, so that water-based drilling fluid inhibition and filtrate reduction properties are improved.
Description
Technical field
The present invention relates to a kind of drilling fluid suppressive starch fluid loss additive and preparation method thereof, relate to oil,
The exploration and development technical field of natural gas and unconventional petroleum resources.
Background technology
Reduce mud shale stratum, in oil/gas drilling process, borehole well instability probability frequently occurs, be to be engaged in oil, sky
So gas resources exploration scientific research personnel's emphasis research direction.From controlling drilling fluid filtration, improving drilling fluid
Inhibition, is the effective means improving this type of stratum wellbore stability.
Starch is the filtrate reducer for drilling fluid product of a class function admirable, has substantial amounts of hydroxyl in its strand,
Can adsorb with stratum clay mineral, adhesion-promoting, the effect such as closure；The dynamic and static of drilling fluid can also be controlled
Filter loss；And almost can be compatible with all water-base drilling fluid inorganic agents.By chemical bond by amido or
Quaternary ammonium salt group introduces in starch molecular chain, prepares cationic starch.Keeping the original filtration reduction of starch
While energy, it is also possible to improve the absorption of starch, rejection, expand it further in drilling fluid simultaneously
Range.
In publication, cationic starch is mainly prepared by etherification method and grafting copolymerization process, its sun from
Sub-property is come as quaternary ammonium salt or cationically polymerizable monomers.By starch reaction centric quantity or the shadow of grafting efficiency
Ring, it is difficult to obtain the starch of high-cation density, therefore cannot give full play to the performance advantage of this series products.
Summary of the invention
It is an object of the invention to provide a kind of drilling fluid suppressive starch fluid loss additive.Anti-at limited starch
In Ying in the heart, introduce many amine compounds, improve starch molecular chain cationic groups in one density, play improvement
Drilling fluid suppression and the purpose of filtration property.
Another object of the present invention is to provide the preparation side of a kind of drilling fluid suppressive starch fluid loss additive
Method, the method, with water as solvent, involved raw material process safety and environmental protection, is prone to industrialization, obtained product
Stable performance.
The technical scheme is that
A kind of drilling fluid suppressive starch fluid loss additive, is prepared from by following raw material, with starch, bridging
Agent and many amine compounds are primary raw material, in deionized water, with reaction system etherified under catalyst action
Standby and obtain；Described bridging agent, catalyst, deionized water quality ratio be, bridging agent: catalyst: go from
Sub-water=1:0.05～0.1:2.5～5；Described starch with many amine compounds mass ratio is, starch: many amidos
Compound=1:1～1.05；Described deionized water with the mass ratio of starch is, deionized water: starch=1:1～2.5.
Described bridging agent be any one in epoxychloropropane, methyl epichlorohydrin, epoxy bromopropane or
Mixture；
Described catalyst is the one in p-methyl benzenesulfonic acid, DBSA, sulfamic acid or mixing
Thing；
Described starch is in carboxymethyl starch sodium, hetastarch, potato starch, soluble starch
Any one or mixture.
Described many amine compounds are polyethylene polyamine, polymine (Mw=300), polymine
(Mw=600), polymine (Mw=1800), polymine (Mw=3500), polymine
(Mw=20000), polymine (Mw=30000), polymine (Mw=50000), polyethylene
Any one in imines (Mw=70000) or mixture.
The preparation method of a kind of drilling fluid suppressive starch fluid loss additive, comprises the following steps:
(1) bridging agent, catalyst, deionized water are joined in four-hole bottle by above-mentioned mass ratio, and by this
Four-hole bottle is fixed on the iron stand with reflux condensation mode, mechanical agitation and temperature regulating device；
(2) start stirring, temperature control and reflux condensate device, set mixing speed as 100～200r/min, temperature
Degree control is 85～95 DEG C, stirring reaction 5～6h；
(3), under stirring, by above-mentioned mass ratio, many amine compounds are poured slowly into step (2) gained
In solution, to maintain temperature be 85～95 DEG C, mixing speed is 200～300r/min, insulated and stirred reaction 3～5h
After, it is cooled to room temperature；
(4), under stirring, by above-mentioned mass ratio, starch is slowly added in step (3) gained solution,
To maintain reactor temperature be 120～130 DEG C, mixing speed is 100～200r/min, insulation reaction 3～5h
After, it is down to room temperature in reactor；
(5) step (4) products therefrom is after 40～50 DEG C of forced air dryings 8～10h, shears pulverizing and obtains powder
Powder material is drilling fluid suppressive starch fluid loss additive of the present invention.
The described bridge in step (1) is connected as epoxychloropropane, methyl epichlorohydrin, epoxy bromopropane
In any one or mixture；
The described catalyst in step (1) is in p-methyl benzenesulfonic acid, DBSA, sulfamic acid
One or mixture；
The described starch in step (3) be carboxymethyl starch sodium, hetastarch, potato starch, can
Any one in soluble starch or mixture.
The described many amine compounds in step (4) be polyethylene polyamine, polymine (Mw=300),
Polymine (Mw=600), polymine (Mw=1800), polymine (Mw=3500),
Polymine (Mw=20000), polymine (Mw=30000), polymine (Mw=50000),
Any one in polymine (Mw=70000) or mixture.
The invention has the beneficial effects as follows:
Suppressive starch fluid loss additive of the present invention is anti-by etherificate by starch, bridging agent and many amine compounds
Should be prepared, its product has on starch molecular chain abundant amine groups, it is possible to clay ore deposit, stratum
The effect of thing generation multipoint adsorption, improves water-base drilling fluid suppression and filtrate loss controllability.
Detailed description of the invention
Specific embodiment is set forth below, so that product of the present invention and preparation process thereof to be described.
Embodiment 1
47.760g epoxychloropropane, 4.776g p-methyl benzenesulfonic acid and 119.400g deionized water are transferred to take back
Flow in the reactor of condensation, temperature control stirring device.Set mixing speed as 100r/min, temperature as 85 DEG C,
Insulation reaction 5h.Maintenance mixing speed is 300r/min, pours in reactor by 47.760g polyethylene polyamine,
Controlling reactor temperature is 85 DEG C, insulation reaction 3h.38.208g carboxymethyl starch sodium is joined
Stating in reactor, adjustment mixing speed is 200r/min, and 120 DEG C of insulation reaction 3h, room temperature is down to by reactor.
Product in reactor is transferred in convection oven, at 40 DEG C after forced air drying 8h, shears pulverizing and obtain powder
Powder material is drilling fluid suppressive starch fluid loss additive of the present invention, is calculated as IF-1.
Embodiment 2
47.760g methyl epichlorohydrin, 2.388g DBSA and 143.280g deionized water turn
Move in the reactor of band reflux condensation mode, temperature control stirring device.Set mixing speed as 200r/min, temperature
It is 95 DEG C, insulation reaction 6h.Maintenance mixing speed is 200r/min, by 50.148g polymine
(Mw=300) pouring in reactor, controlling reactor temperature is 95 DEG C, insulation reaction 5h.By 42.984
G hetastarch joins in aforesaid reaction vessel, and adjustment mixing speed is 100r/min, 130 DEG C of insulation reaction
5h, room temperature is down to by reactor.Product in reactor is transferred in convection oven, forced air drying 10 at 50 DEG C
After h, shearing pulverizing obtains powdered substance and is drilling fluid suppressive starch fluid loss additive of the present invention, is calculated as
IF-2。
Embodiment 3
47.760g epoxy bromopropane, 4.000g sulfamic acid and 130.500g deionized water are transferred to band backflow
Condensation, temperature control stirring device reactor in.Set mixing speed as 150r/min, temperature as 90 DEG C, guarantor
Temperature reaction 4h.Maintenance mixing speed is 250r/min, by 49.500g polymine under stirring
(Mw=600) pouring in reactor, controlling reactor temperature is 90 DEG C, insulation reaction 4h.By 20.500
G carboxymethyl starch sodium and 20.000g hetastarch join in aforesaid reaction vessel, adjust mixing speed and are
150r/min, 125 DEG C of insulation reaction 4h, room temperature is down to by reactor.Product in reactor is transferred to air blast
In baking oven, at 50 DEG C after forced air drying 9h, shearing pulverizing obtains powdered substance and is drilling fluid of the present invention
With suppressive starch fluid loss additive, it is calculated as IF-3.
Embodiment 4～9
The described step of embodiment 4～9 such as embodiment 1, needed raw material proportioning and reaction condition are shown in Table 1 and table
2。
The present invention compared with prior art have the advantage that and effect are as follows by verification experimental verification:
Saturated salt-water drilling fluid: add 8g soda and 100g calcium bentonite in 1000mL tap water is high
Speed stirring 20min, room temperature stands after placing 48h, then is added thereto to the sodium chloride of 36%, high-speed stirred
10min, room temperature stands places 16h, obtains saturated salt-water drilling fluid.
Adding product I F-1 of the present invention, IF-2, IF-3 in the above-mentioned drilling fluid of 350mL, 150 DEG C roll old
After changing 16h, the High Temperature High Pressure dehydration filter loss of test drilling fluid.
It is as follows that landwaste rolls recovery experiment step:
(1) measure 1% product I F-1 of the present invention, IF-2, IF-3 in 350mL clear water, high-speed stirred
5min is standby；
(2), after particle diameter landwaste between 2.0～5.0mm is dried 4h at 103 DEG C, it is down to room temperature
Standby；
(3) weigh the above-mentioned landwaste of 20g and put into ageing can, and pour clear water into；
(4), after above-mentioned ageing can seals, take out after rolling 16h cooling at 150 DEG C.Use aperture 0.42mm
Sieve reclaims landwaste, and is dried 4h at 103 DEG C, is down to room temperature and weighs recovery landwaste quality；
(5) shale recovery ratio R is calculated according to formula 1.
R=G1/G0× 100% (formula 1)
In formula:
G0: shale quality, g
G1: the shale quality after recovery, g
R: shale recovery ratio, %
Portioned product filtrate loss controllability of the present invention and landwaste roll recyclability evaluation result and are shown in Table 3, table 3
Middle high temperature and high pre ssure filtration test temperature is 150 DEG C, and "--" expression is not tested, and result above shows, this
Bright drilling fluid suppressive starch fluid loss additive, it is possible to improve the High Temperature High Pressure filtration property of drilling fluid, meanwhile,
The rolling response rate of shale is reached more than 90%, and temperature resistance is up to 150 DEG C.
Table 1 embodiment 4～9 step (1)～the proportioning raw materials of (2) and reaction condition
Table 2 embodiment 4～9 step (3)～the proportioning raw materials of (5) and reaction condition
Table 3 filtrate loss controllability and shale roll the response rate
Claims (10)
1. a drilling fluid suppressive starch fluid loss additive, it is characterised in that be prepared from by following raw material, with starch, bridging agent and many amine compounds as primary raw material, in deionized water, is prepared with reaction etherified under catalyst action；Described bridging agent, catalyst, deionized water quality ratio be, bridging agent: catalyst: deionized water=1:0.05 ~ 0.1:2.5 ~ 5；Described starch with many amine compounds mass ratio is, starch: many amine compound=1:1 ~ 1.05；Described deionized water with the mass ratio of starch is, deionized water: starch=1:1 ~ 2.5.
A kind of drilling fluid suppressive starch fluid loss additive the most according to claim 1, it is characterised in that described bridging agent is any one in epoxychloropropane, methyl epichlorohydrin, epoxy bromopropane or mixture.
A kind of drilling fluid suppressive starch fluid loss additive the most according to claim 1, it is characterised in that described catalyst is the one in p-methyl benzenesulfonic acid, DBSA, sulfamic acid or mixture.
A kind of drilling fluid suppressive starch fluid loss additive the most according to claim 1, it is characterised in that described starch is any one in carboxymethyl starch sodium, hetastarch, potato starch, soluble starch or mixture.
A kind of drilling fluid suppressive starch fluid loss additive the most according to claim 1, it is characterised in that described many amine compounds are any one in polyethylene polyamine, polymine (Mw=300), polymine (Mw=600), polymine (Mw=1800), polymine (Mw=3500), polymine (Mw=20000), polymine (Mw=30000), polymine (Mw=50000), polymine (Mw=70000) or mixture.
The preparation method of a kind of drilling fluid suppressive starch fluid loss additive the most according to claim 1, it is characterised in that comprise the following steps:
(1) bridging agent, catalyst, deionized water are joined in four-hole bottle by above-mentioned mass ratio, and this four-hole bottle is fixed on the iron stand with reflux condensation mode, mechanical agitation and temperature regulating device；
(2) starting stirring, temperature control and reflux condensate device, set mixing speed as 100 ~ 200 r/min, it is 85 ~ 95 DEG C that temperature controls, and stirs reaction 5 ~ 6 h；
(3) under stirring, being poured slowly in step (2) gained solution by many amine compounds by above-mentioned mass ratio, to maintain temperature be 85 ~ 95 DEG C, mixing speed is 200 ~ 300 r/min, after insulated and stirred reaction 3 ~ 5 h, is cooled to room temperature；
(4) under stirring, being slowly added in step (3) gained solution by starch by above-mentioned mass ratio, to maintain reactor temperature be 120 ~ 130 DEG C, mixing speed is 100 ~ 200 r/min, after insulation reaction 3 ~ 5 h, is down to room temperature in reactor；
(5) step (4) products therefrom is after 40 ~ 50 DEG C of forced air drying 8 ~ 10 h, and shearing pulverizing obtains powdered substance and is drilling fluid suppressive starch fluid loss additive of the present invention.
The preparation method of a kind of drilling fluid suppressive starch fluid loss additive the most according to claim 6, it is characterised in that the described bridge in step (1) is connected as any one in epoxychloropropane, methyl epichlorohydrin, epoxy bromopropane or mixture.
The preparation method of a kind of drilling fluid suppressive starch fluid loss additive the most according to claim 6, it is characterised in that the described catalyst in step (1) is the one in p-methyl benzenesulfonic acid, DBSA, sulfamic acid or mixture.
The preparation method of a kind of drilling fluid suppressive starch fluid loss additive the most according to claim 6, it is characterised in that the described starch in step (3) is any one in carboxymethyl starch sodium, hetastarch, potato starch, soluble starch or mixture.
The preparation method of a kind of drilling fluid suppressive starch fluid loss additive the most according to claim 6, it is characterised in that the described many amine compounds in step (4) are any one in polyethylene polyamine, polymine (Mw=300), polymine (Mw=600), polymine (Mw=1800), polymine (Mw=3500), polymine (Mw=20000), polymine (Mw=30000), polymine (Mw=50000), polymine (Mw=70000) or mixture.
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107090281A (en) * | 2017-05-05 | 2017-08-25 | 辽宁石油化工大学 | A kind of preparation method of drilling fluid mobile phase |
| CN107815927A (en) * | 2017-09-29 | 2018-03-20 | 当涂县瑞龙果树种植专业合作社 | A kind of Environmental-protection agricultural paper mulch sheet with enhanced water resistance energy and preparation method thereof |
| CN108219759A (en) * | 2018-01-22 | 2018-06-29 | 中国石油大学(华东) | A kind of preparation method of branching type water-base drilling fluid fluid loss additive |
| CN108715756A (en) * | 2018-07-20 | 2018-10-30 | 中国石油集团川庆钻探工程有限公司工程技术研究院 | A kind of modified starch filtration-control additive and its preparation method and application |
| CN108949122A (en) * | 2018-06-14 | 2018-12-07 | 中国石油集团工程技术研究院有限公司 | A kind of heat resisting fluid loss reducing agent and preparation method thereof |
| CN108997508A (en) * | 2017-06-06 | 2018-12-14 | 中国石油化工股份有限公司 | A kind of drilling fluid modified starch anti-sloughing agent and preparation method thereof |
| CN109420469A (en) * | 2017-08-22 | 2019-03-05 | 中国石油化工股份有限公司 | A kind of cation doping spherex material and its preparation method and application |
| CN109666470A (en) * | 2018-12-05 | 2019-04-23 | 延安中杰高新工贸有限公司 | A kind of compound profile-controlling and plugging agent of nano and micro materials |
| CN114479782A (en) * | 2020-10-27 | 2022-05-13 | 中国石油化工股份有限公司 | Plugging agent and preparation method and application thereof |
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107090281A (en) * | 2017-05-05 | 2017-08-25 | 辽宁石油化工大学 | A kind of preparation method of drilling fluid mobile phase |
| CN108997508A (en) * | 2017-06-06 | 2018-12-14 | 中国石油化工股份有限公司 | A kind of drilling fluid modified starch anti-sloughing agent and preparation method thereof |
| CN108997508B (en) * | 2017-06-06 | 2021-12-28 | 中国石油化工股份有限公司 | Modified starch anti-sloughing agent for drilling fluid and preparation method thereof |
| CN109420469A (en) * | 2017-08-22 | 2019-03-05 | 中国石油化工股份有限公司 | A kind of cation doping spherex material and its preparation method and application |
| CN107815927A (en) * | 2017-09-29 | 2018-03-20 | 当涂县瑞龙果树种植专业合作社 | A kind of Environmental-protection agricultural paper mulch sheet with enhanced water resistance energy and preparation method thereof |
| CN108219759A (en) * | 2018-01-22 | 2018-06-29 | 中国石油大学(华东) | A kind of preparation method of branching type water-base drilling fluid fluid loss additive |
| CN108219759B (en) * | 2018-01-22 | 2019-01-01 | 中国石油大学(华东) | A kind of preparation method of branching type water-base drilling fluid fluid loss additive |
| CN108949122A (en) * | 2018-06-14 | 2018-12-07 | 中国石油集团工程技术研究院有限公司 | A kind of heat resisting fluid loss reducing agent and preparation method thereof |
| CN108715756A (en) * | 2018-07-20 | 2018-10-30 | 中国石油集团川庆钻探工程有限公司工程技术研究院 | A kind of modified starch filtration-control additive and its preparation method and application |
| CN109666470A (en) * | 2018-12-05 | 2019-04-23 | 延安中杰高新工贸有限公司 | A kind of compound profile-controlling and plugging agent of nano and micro materials |
| CN114479782A (en) * | 2020-10-27 | 2022-05-13 | 中国石油化工股份有限公司 | Plugging agent and preparation method and application thereof |
| CN114479782B (en) * | 2020-10-27 | 2023-05-26 | 中国石油化工股份有限公司 | Plugging agent and preparation method and application thereof |
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Application publication date: 20160817 |