CN110372804A - Anti-salt temperature-resistant starch drilling well fluid loss additive and preparation method thereof - Google Patents
Anti-salt temperature-resistant starch drilling well fluid loss additive and preparation method thereof Download PDFInfo
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- CN110372804A CN110372804A CN201910634537.6A CN201910634537A CN110372804A CN 110372804 A CN110372804 A CN 110372804A CN 201910634537 A CN201910634537 A CN 201910634537A CN 110372804 A CN110372804 A CN 110372804A
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- 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
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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
- C09K8/03—Specific additives for general use in well-drilling compositions
- C09K8/035—Organic additives
Abstract
The invention discloses a kind of anti-salt temperature-resistant starch drilling well fluid loss additives and preparation method thereof, it is related to the technical field of fluid loss additive, formula includes the component of following parts by weight: 100-125 parts of starch, 30-60 parts of expanding treatment agent, 10-20 parts of sodium hydroxide, 25-50 parts of monoxone, wherein expanding treatment agent includes alum and sodium bicarbonate；The anti-salt temperature-resistant starch drilling well fluid loss additive and preparation method thereof is the following steps are included: S1. pretreatment of starch, the alkalization of S2. starch, S3. starch etherificate, S4. dispersion drying.The present invention has the technical effect that anti-saturation salt outlet capacity is strong, temperature tolerance is good.
Description
Technical field
The present invention relates to the technical field of fluid loss additive, more particularly, to anti-salt temperature-resistant starch drilling well fluid loss additive and its
Preparation method.
Background technique
Drilling fluid is one of maximum oil field chemical of dosage, and fluid loss additive is then very important one kind in drilling fluid
Additive.The loss that drilling fluid is not only resulted in when drilling fluid filtration is excessive, also results in cave-in, and pollution reservoir etc. is tight
Weight consequence.Fluid loss additive is mainly the flexible thin and compact filter cake by forming low-permeability on the borehole wall, hence it is evident that reduces and bores
Well liquid filter loss, the borehole wall of safeguarding stability, it is ensured that drilling well can be carried out quickly and safely.However rock salt, the mud of some high salty formations
Cream rock fascicule thickness is up to 1500 meters or more, and deep-well big (well depth is mostly at 3000 meters or more), downhole temperature are high, are applicable in
Mud system is saturated brine system, it requires mud materials saline-alkaline tolerance with higher.
Traditional fluid loss additive is mostly water-soluble high-molecular compound, and matrix mainly uses natural polymer, such as day
Right cellulose, starch, humic acid or some modified natural polymer materials.Wherein starch fluid loss additive mainly uses pre- glue
Change starch, pregelatinized starch realizes that filtrate reducing acts on by the blocking that grid structure stablizes clay particle and aquation macromolecular.But
It is that these common natural polymers or flocculation fluid loss additive are difficult to meet the saturated brine system of saliferous strata
Required mud system performance requirement.
Summary of the invention
The purpose of the present invention one is to provide the anti-salt temperature-resistant starch drilling well that a kind of anti-saturation salt outlet capacity is strong, temperature tolerance is good
Fluid loss additive, the purpose of the present invention two are to provide the preparation method of the anti-salt temperature-resistant starch drilling well fluid loss additive.
The technical scheme is that:
A kind of anti-salt temperature-resistant starch drilling well fluid loss additive, the component including following parts by weight:
Wherein expanding treatment agent includes alum and sodium bicarbonate.
By using above-mentioned technical proposal, alum and sodium bicarbonate reaction in expanding treatment agent generate carbon dioxide gas,
Carbon dioxide gas penetrates between starch polymer, destroys the crystalline texture of starch and reduces the interaction between starch molecule
Power makes starch become soft fluffy state from dense state.This bulked structure is the extruding on microcosmic, between increasing between starch molecule
Away to sufficiently expose the hydroxyl group sites that may participate in reaction in starch.
Starch is first reacted with sodium hydroxide generation threading after expanding treatment in formula generates activated centre sodium starch,
Reaction equation are as follows: starch-OH+NaOH → starch-ONa (activated centre)+H20(1-1)；Then sodium starch and the chlorine as etherifying agent
Etherification reaction occurs for acetic acid, and monoxone becomes sodium chloroacetate, reaction equation under alkaline environment are as follows: starch-ONa+ClCH2COONa+
NaOH → starch-O-CH2COONa+NaCl+H2O(1-2).The hydroxyl group sites being sufficiently exposed in sodium hydroxide and starch are reacted
Become activated centre, sodium chloroacetate penetrates into the intermolecular distance inside expanded starch particle, the work with exposure in expanded starch
Change central contact, therefore etherification reaction resistance is smaller, reaction rate and etherificate degree are higher, overcome traditional starch filtrate reducing
Agent is etherified the low problem of degree of substitution.Starch etherificate degree is higher, and the haloacetate group introduced in starch is more, to preferably change
The temperature-resistant anti-salt performance of kind starch, modified starch fluid loss additive can meet needed for the saturated brine system of saliferous strata
Mud system performance requirement.
Be further arranged to: the weight fraction ratio of alum and sodium bicarbonate is 2:1 in the expanding treatment agent.
By using above-mentioned technical proposal, reaction equation that alum and sodium bicarbonate react are as follows: 2KAl (SO4)2·12H20+
6NaHCO3→K2SO4+3Na2SO4+2Al(OH)3↓+6CO2↑(1-3)；By reaction equation (1-3) it is found that alum is reacted with sodium bicarbonate
When the ratio between the amount of substance that consumes be 1:3, the mass ratio that corresponding alum consumes when reacting with sodium bicarbonate is approximately 1.88:1.When
When the weight fraction ratio of alum and sodium bicarbonate is 2:1, i.e., alum is excessive, thus by sodium bicarbonate fully reacting, production as much as possible
Raw CO2Gas makes the abundant extruding of starch granules, in the intermolecular distance for being easier sodium chloroacetate penetrate into inside starch granules,
Improve etherificate rate and etherificate degree.
Be further arranged to: the monoxone is crystalline powder, and the sodium hydroxide is chip solid.
By using above-mentioned technical proposal, the monoxone of crystalline powder and the sodium hydroxide of chip solid are sent out on the spot when contacting
Raw neutralization reaction, generates sodium chloroacetate and water.The heat of neutralization reaction heat release, releasing further unlocks starch molecular chain.And
It is not aqueous in reaction system since monoxone and sodium hydroxide are solid-solid reactions, therefore neutralization reaction not as good as swashing in aqueous solution
Strong, the rate of reaction heat release can be effectively controlled, and Exotherm Time is extended, this feature can effectively reduce heat release concentration
Unfavorable side reaction under Shi Gaowen occurs, and extended Exotherm Time is then conducive to the activated centre of sodium chloroacetate and starch granules
Reaction carries out, and improves etherificate efficiency.
A kind of preparation method of anti-salt temperature-resistant starch drilling well fluid loss additive, comprising the following steps:
S1. pretreatment of starch: starch is stirred under room temperature, expanding treatment agent is added into starch, is uniformly mixed to obtain extruding
Starch；
S2. starch alkalizes: sodium hydroxide is added into expanded starch obtained in S1 step, is uniformly mixing to obtain alkalization starch；
S3. starch is etherified: monoxone is added in the alkalization starch into S2 step while stirring, fully reacting obtains carboxymethyl shallow lake
Powder；
S4. disperse drying: carboxymethyl starch obtained in S3 step is dried, obtain finished product fluid loss additive.
By using above-mentioned technical proposal, in S1 step, expanding treatment agent is first put into starch, makes expanding treatment agent pair
Starch carries out expanding treatment, and the carbon dioxide gas that expanding treatment agent reaction generates can be penetrated into effectively between starch polymer,
Intermolecular interaction force is reduced, the crystalline texture of starch is destroyed, so that starch becomes puffy from closely knit shape, obtains extruding
Starch granules.Make the hydroxyl group sites of starch granules sufficiently exposure reaction simultaneously, exposed hydroxyl group sites can be in S2 step
Can more easily carry out reacting with solid sodium hydroxide and generate activated centre sodium starch, and with activated centre sodium starch phase
The sodium chloroacetate of mutual reactance can effectively be penetrated into inside starch granules in the state of being not required to starch gelatinization and be contacted with hydroxyl,
Effectively etherificate is implemented to starch, obtains high degree of substitution.
This process uses nearly dry technology for production, using monoxone and sodium hydroxide reaction process exothermic thermal energy from
So heating, and be not required to dissolution neutralize, centrifugation, do not have to solvent, without subsequent baking process, energy consumption less, wastewater discharge it is few, produce
The cost of product is low, and avoids the shortcomings that low degree of substitution, the product that solid phase etherification reaction faces cannot reach the performance of requirement；Separately
On the one hand, this technique also has the advantages of gelatinization technique, i.e., starch molecule is sufficiently spread out, and is conducive to the raising of reaction efficiency, energy
Degree of substitution is effectively improved, the haloacetate group introduced in starch is more, thus preferably improve the temperature-resistant anti-salt performance of starch, and
And the disadvantages of avoiding the high energy consumption of gelatinization technique, energy conservation and environmental protection are all had a very important significance.
Be further arranged to: in the S1 step, expanding treatment agent, the charging of expanding treatment agent is added in starch while stirring
Speed v is 1-1.2 parts/min, and mixing time t1 is 30-50min.
Be further arranged to: in the S3 step, the reaction time t2 of monoxone and alkalization starch is 60-120min.
By using above-mentioned technical proposal, expanding treatment agent is added in starch while stirring, and expanding treatment agent is with 1-1.2
The speed of part/min is slowly added into starch, and expanding treatment agent and starch can be made to be sufficiently mixed the titanium dioxide for making to generate
Carbon gas sufficiently carries out extruding to starch granules, improves the extruding efficiency of expanding treatment agent, increases starch swelling degree, Jin Erti
High etherificate degree of substitution, conducive to the temperature-resistant anti-salt performance of enhancing starch.In S3 step, the first hydroxide with alkalization starch of monoxone
Sodium occurs neutralization reaction and generates sodium chloroacetate, then anti-by the activated centre sodium starch generation etherificate in sodium chloroacetate and alkalization starch
It answers, the reaction time of monoxone and alkalization starch is 60-120min, chloroacetic two-step reaction can be made more sufficiently thoroughly,
Improve etherificate efficiency and etherificate quality.
Be further arranged to: in the S4 step, cold water drop is first added in carboxymethyl starch thereto before drying
It warms to room temperature, then is dried.
By using above-mentioned technical proposal, since neutralization reaction, reaction occur for monoxone and sodium hydroxide in the S3 step
Heat release, therefore carboxymethyl starch temperature obtained in S3 step is all higher, if drying carboxymethyl starch at relatively high temperatures, holds
It easily is gelatinized carboxymethyl starch, the temperature-resistant anti-salt performance of carboxymethyl starch is caused to decline, therefore, carboxymethyl is formed sediment with cold water
Powder is dried again after being cooled to room temperature, and the carboxymethyl starch class fluid loss additive generated can be made to keep preferable temperature-resistant anti-salt
Property.
It is further arranged to: in the S4 step, after carboxymethyl starch is cooled to room temperature, investment dispersant dispersion
30min, then be dried.
Add by using above-mentioned technical proposal since carboxymethyl starch is cooled to room temperature with cold water before drying
Carboxymethyl starch particle is easy to agglomerate due to reunion after entering cold water, and dispersing agent is put into carboxymethyl starch makes carboxymethyl
Starch granules dispersion is complete, convenient for improving the service performance of later period carboxymethyl starch.
In conclusion advantageous effects of the invention are as follows:
(1) before starch and monoxone carry out etherification reaction, extrusion pretreatment is carried out to starch first with expanding treatment agent, is made
Starch becomes soft fluffy state from dense state, and sufficiently exposes the hydroxyl group sites that may participate in reaction in starch, and sodium hydroxide can be with
It is more easily reacted with hydroxyl group sites and generates activated centre sodium starch, so that the etherification reaction for reducing sodium chloroacetate and starch hinders
Power improves starch and is etherified degree, introduces more haloacetate groups, to preferably improve the temperature-resistant anti-salt performance of starch；
(2) it is heated up naturally using the exothermic thermal energy of monoxone and sodium hydroxide reaction process, and be not required to dissolve and neutralize, be centrifuged,
Without solvent, without subsequent baking process, energy consumption less, wastewater discharge is few, product cost is low, and avoid solid phase etherificate
React the shortcomings that low degree of substitution, the product faced cannot reach the performance of requirement；
(3) after etherification reaction generates carboxymethyl starch, carboxymethyl starch is cooled to room temperature using cold water and dispersed again, do
It is dry, it can occur at relatively high temperatures to be gelatinized to avoid carboxymethyl starch and agglomerate, keep the drop filter of carboxymethyl starch class to stablize
Losing agent has preferable heat and salt resistance.
Specific embodiment
A kind of embodiment 1: anti-salt temperature-resistant starch drilling well fluid loss additive, recipe ingredient and its content as shown in table 1 (1
Parts by weight=1kg or 1 parts by weight=1g), the present embodiment is by taking 1 parts by weight=1g as an example.Wherein starch is formed sediment using corn
Powder, monoxone are crystalline powder, and sodium hydroxide is chip solid.The preparation process of the anti-salt temperature-resistant starch drilling well fluid loss additive
The following steps are included:
S1. pretreatment of starch: adding starch into reaction kneader under room temperature, while stirring into starch with v=1-1.2 parts/
The speed of min adds expanding treatment agent, and remains that the addition weight part ratio of alum and sodium bicarbonate is 2:1, when stirring
Between t1 be 30min until be uniformly mixed to obtain expanded starch；
S2. starch alkalizes: sodium hydroxide is added into expanded starch obtained in S1 step, is uniformly mixing to obtain alkalization starch；
S3. starch is etherified: monoxone is added in the alkalization starch into S2 step and is stirred, mixing time t2 is 60min,
Carboxymethyl starch is obtained to the abundant fully reacting of monoxone；
S4. disperse drying: into carboxymethyl starch obtained in S3 step be added cold water until carboxymethyl starch be cooled to room temperature,
Dispersing agent is added into carboxymethyl starch again and disperses 30min, (natural air drying) is dried in carboxymethyl starch after discharging, is obtained
Finished product fluid loss additive.
1 embodiment 1-5 recipe ingredient of table and its content table (1 parts by weight=1kg)
Embodiment 2: a kind of anti-salt temperature-resistant starch drilling well fluid loss additive, the present embodiment the difference from embodiment 1 is that,
Recipe ingredient and its content are (1 parts by weight=1kg) as shown in table 1, t1 35min, t2 75min.
Embodiment 3: a kind of anti-salt temperature-resistant starch drilling well fluid loss additive, the present embodiment the difference from embodiment 1 is that,
Recipe ingredient and its content are (1 parts by weight=1kg) as shown in table 1, t1 40min, t2 90min.
Embodiment 4: a kind of anti-salt temperature-resistant starch drilling well fluid loss additive, the present embodiment the difference from embodiment 1 is that,
Recipe ingredient and its content are (1 parts by weight=1kg) as shown in table 1, t1 45min, t2 105min.
Embodiment 5: a kind of anti-salt temperature-resistant starch drilling well fluid loss additive, the present embodiment the difference from embodiment 1 is that,
Recipe ingredient and its content are (1 parts by weight=1kg) as shown in table 1, t1 50min, t2 120min.
Comparative example 1: this comparative example the difference from embodiment 1 is that, in the formula of this comparative example do not contain expanding treatment agent,
Correspondingly, pretreatment of starch step is not contained in preparation step.
Comparative example 2: this comparative example is distinguished with embodiment 1 to be, the weight fraction ratio of alum and sodium bicarbonate in this comparative example
For 1:1.
Comparative example 3: this comparative example the difference from embodiment 1 is that, t1 10min.
Comparative example 4: this comparative example the difference from embodiment 1 is that, t1 70min.
Comparative example 5: this comparative example the difference from embodiment 1 is that, t2 30min.
Comparative example 6: this comparative example the difference from embodiment 1 is that, t2 150min.
Performance test:
(1) the high temperature resistant property experimental formula of fresh water-based slurry and method are as follows:
Formula :+3% anti-salt temperature-resistant starch drilling well fluid loss additive of 6% fresh water-based slurry.6g bentonite is added in i.e. every 100mL water
Fresh water-based slurry is made, is then separately added into anti-salt temperature-resistant prepared in 3g embodiment 1-5, comparative example 1-6 in every 100mL base slurry
Starch drilling well fluid loss additive measures API filtration after conserving 16h under the conditions of 230 DEG C, and experimental result is as shown in table 2.
The mud filtration amount of the fresh water-based slurry of 2 embodiment 1-5 of table, comparative example 1-6 preparation
(2) the Experiment of salt-resisting performance of polyvinyl formula of supersaturated brine base slurry and method are as follows:
Formula: 5% base starches+4% anti-salt temperature-resistant starch drilling well fluid loss additive+sodium chloride.5g swelling is added in i.e. every 100mL water
Supersaturated brine base slurry is made in soil, excess chlorination sodium, is then separately added into 3g embodiment 1- in every 100mL supersaturated brine base slurry
5, anti-salt temperature-resistant starch drilling well fluid loss additive prepared in comparative example 1-6 measures API after conserving 16h under the conditions of 230 DEG C
Filter loss, experimental result are as shown in table 3.Experimental result is as shown in table 3.
The mud filtration amount of the supersaturated brine base slurry of 3 embodiment 1-5 of table, comparative example 1-6 preparation
Data analysis:
Analytical table 2, from the data in table 2, it can be seen that mud filtration amount base of the fresh water-based slurry of embodiment 1-5 preparation under the conditions of 230 DEG C
Originally it is maintained at 4-6mL, illustrates the anti-salt temperature-resistant starch drilling well fluid loss additive of embodiment 1-5 preparation in 230 DEG C of items of fresh water-based slurry
Index request is fully achieved under part, there is control dehydration effect well；
The API filtration of comparative example 1 reaches 54.8, illustrates that the starch in comparative example 1 is pre- without expanding treatment agent progress extruding
Processing, causes the etherificate degree of substitution of starch smaller, and the filtrate reducing ability for eventually leading to fluid loss additive reduces；
The API filtration of comparative example 2 is 32.4, lower than the API filtration of comparative example 1 but be still higher than index value, illustrates to work as extruding
When the weight fraction ratio of alum and sodium bicarbonate in inorganic agent is 1:1, that is, sodium bicarbonate excess, the not sufficiently reactive production two of sodium bicarbonate
Carbonoxide carries out abundant extruding to starch in turn, eventually leads to the heatproof filtrate reducing ability decline of fluid loss additive；
The API filtration of comparative example 3 is 12.5, lower than comparative example 1 and comparative example 2, but still higher than the filter loss of embodiment 1-5,
Illustrate that the mixing time of expanding treatment agent and starch has an impact to the performance of fluid loss additive in comparative example 3, which embodies
For the mixing time of expanding treatment agent and starch is too short, makes the inabundant extruding of starch, leads to the subsequent etherificate degree of substitution drop of starch
It is low, eventually lead to the heatproof control dehydration performance decline of fluid loss additive；
The API filtration of comparative example 4 is 6.4, illustrates that the mixing time of expanding treatment agent and starch is too long, to the property of fluid loss additive
It can influence less, but increase the production cycle of fluid loss additive, be unfavorable for enterprise and efficiently produce；
The API filtration of comparative example 5 is 17.2, illustrates that alkalization starch and chloroacetic reaction time are too short, will lead to alkalization and forms sediment
The etherificate of powder is incomplete, eventually leads to the high-temperature control dehydration performance decline of fluid loss additive.
Analytical table 3, the saturated salt of embodiment 1-5 preparation water base slurry mud 230 DEG C under the conditions of similar with above-mentioned analysis
Filter loss substantially remains in 5mL or so, illustrates the anti-salt temperature-resistant starch drilling well fluid loss additive of embodiment 1-5 preparation in saturated salt
Index request is fully achieved under the conditions of water base 230 DEG C of slurry, there is control dehydration effect well；Comparative example 1-6 with above-mentioned point
Analyse similar, this will not be repeated here.
The implementation principle of the present embodiment and have the beneficial effect that using expanding treatment agent to starch carry out extrusion pretreatment, fill
Divide the hydroxyl group sites reacted in exposure starch granules, the solid-state sodium chloroacetate for generating solid NuaO and chloroacetate reaction can
It is contacted with effectively penetrating into inside starch granules with hydroxyl group sites, starch is efficiently etherified, the heatproof of fluid loss additive is improved
Anti-salt property is improved by a relatively large margin；The advantages of also utilizing conventional solid reaction simultaneously: solvent is not had to, without subsequent baking
Dry process, energy consumption are less, wastewater discharge is few, product cost is low, and have the low degree of substitution for avoiding solid phase etherification reaction and facing,
Product cannot reach the shortcomings that performance of requirement.
The embodiment of present embodiment is presently preferred embodiments of the present invention, not limits protection of the invention according to this
Range, therefore: the equivalence changes that all structures under this invention, shape, principle are done, should all be covered by protection scope of the present invention it
It is interior.
Claims (8)
1. a kind of anti-salt temperature-resistant starch drilling well fluid loss additive, which is characterized in that the component including following parts by weight:
100-125 parts of starch；
30-60 parts of expanding treatment agent；
10-20 parts of sodium hydroxide；
25-50 parts of monoxone；
Wherein expanding treatment agent includes alum and sodium bicarbonate.
2. anti-salt temperature-resistant starch drilling well fluid loss additive according to claim 1, it is characterised in that: the expanding treatment agent
The weight fraction ratio of middle alum and sodium bicarbonate is 2:1.
3. anti-salt temperature-resistant starch drilling well fluid loss additive according to claim 2, it is characterised in that: the monoxone is crystalline substance
Sprills, the sodium hydroxide are chip solid.
4. a kind of preparation method of the anti-salt temperature-resistant starch drilling well fluid loss additive as described in claim 1-3, including following step
It is rapid:
S1. pretreatment of starch: starch is stirred under room temperature, expanding treatment agent is added into starch, is uniformly mixed to obtain extruding
Starch；
S2. starch alkalizes: sodium hydroxide is added into expanded starch obtained in S1 step, is uniformly mixing to obtain alkalization starch；
S3. starch is etherified: monoxone is added in the alkalization starch into S2 step, fully reacting obtains carboxymethyl starch；
S4. disperse drying: carboxymethyl starch obtained in S3 step is dried, obtain finished product fluid loss additive.
5. the preparation method of anti-salt temperature-resistant starch drilling well fluid loss additive according to claim 4, it is characterised in that: described
In S1 step, starch is added expanding treatment agent while stirring, and the charging rate v of expanding treatment agent is 1-1.2 parts/min, when stirring
Between t1 be 30-50min.
6. the preparation method of anti-salt temperature-resistant starch drilling well fluid loss additive according to claim 4 or 5, it is characterised in that:
In the S3 step, the reaction time t2 of monoxone and alkalization starch is 60-120min.
7. the preparation method of anti-salt temperature-resistant starch drilling well fluid loss additive according to claim 4, it is characterised in that: described
In S4 step, carboxymethyl starch is first added cold water thereto before drying and is cooled to room temperature, then is dried.
8. the preparation method of anti-salt temperature-resistant starch drilling well fluid loss additive according to claim 7, it is characterised in that: described
In S4 step, after carboxymethyl starch is cooled to room temperature, investment dispersant disperses 30min, then is dried.
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| CN116589601A (en) * | 2023-05-22 | 2023-08-15 | 山东一滕新材料股份有限公司 | Hydroxypropyl starch, preparation method thereof, modified hydroxypropyl starch and application thereof |
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Application publication date: 20191025 |