CN104418984B - High-temperature resistant clay stabilizer and preparation method thereof - Google Patents
High-temperature resistant clay stabilizer and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a high-temperature resistant clay stabilizer and a preparation method thereof. The preparation method comprises the following steps: carrying out initiation reaction on epoxy chloropropane, dimethylamine and unsaturated quaternary ammonium salt with a sulfonate-containing anionic monomer under a certain condition; and then adding a chain transfer agent in the reaction process to control the molecular weight and after reaction, obtaining the clay stabilizer, wherein both the main and side chains contain cations and the side chain further contains anions. The clay stabilizer has the abilities of resisting temperature, preventing salt and resisting pollution; the clay stabilizer is small in use level, scouring resistant and good in anti-swelling effect; and the molecular weight is ranged from 1500 to 6000, so that the high-temperature resistant clay stabilizer is suitable for a low permeability reservoir.
Description
Technical field
The present invention relates to a kind of high temperature resistant clay stabilizer and preparation method thereof.
Background technology
Contain a certain amount of clay mineral in stratum, mainly have kaolinite, montmorillonite, illite and chlorite etc., in oil
Field development process（Water filling, acidifying, pressure break）Will expand when these clays run into secondary water or water-based material, disperse,
Migration, blocking hole throat, cause in-place permeability to reduce, and destroy even more serious for hypotonic rate oil reservoir.In order to mitigate to storage
Layer injury, is commonly incorporated into clay stabilizer to improve hydration swelling, the dispersion migration of clay in oil field.
Can be divided into according to the different clay stabilizers of chemical constitution：Inorganic salts, inorganic many nuclear polymers class, You Jiju
Compound class.
Inorganic salts clay stabilizer has cheap, and short-term preventive effect of expansion is good；Shortcoming is can not to form multipoint adsorption,
Timeliness is short.
Inorganic many nuclear polymers class mainly has hydroxy Al, zirconyl hydroxy, iron carbonyl etc..This kind of clay stabilizer can effectively prevent
Clay swell and migration, but acid resistance difference is it is impossible to be used for the high sandstone formation of carbonate content.
Organic polymer species are to study a most commonly used class clay stabilizer.At present, this kind of clay stabilizer is using
Many for organic cation type polymer.This kind of clay stabilizer again based on polyquarternium-type, such as：Poly dimethyl allyl
Ammonium chloride, poly- trimethylallylammonium chloride, PAMC etc..Such clay stabilizer have heatproof, acidproof, have
The advantages of effect phase is long.The organic clay stabilizerses using at present are most to be straight chain type, easy centering low permeability formation when molecular weight is big
Hole throat results in blockage, and molecular weight hour preventive effect of expansion is poor, and effect duration is short.
Although existing clay stabilizer has the ability of heatproof, clay stabilization to a certain extent, high temperature resistant,
Salt resistance, long-lasting and in middle LOW PERMEABILITY RESERVOIR use Shortcomings.
Content of the invention
For the deficiencies in the prior art, it is an object of the invention to provide a kind of high temperature resistant clay stabilizer and its preparation work
Skill.
The technical solution used in the present invention is：High temperature resistant clay stabilizer is it is characterised in that this stabilizer is by epoxy chlorine
Propane, dimethylamine, unsaturated quaternary ammonium salt are polymerized with containing sulfonic monomer, and its main chain contains azonia, and its side
Chain contains azonia and azochlorosulfonate acid anion simultaneously.
Described clay stabilizer is it is characterised in that its molecular structural formula is as follows：
In formula, x：y：z=（1-42）：（1-14）：（1-10）；
Or its molecular structural formula is as follows：
In formula, x：y：z=（1-42）：（1-12）：（1-12）；
Or its molecular structural formula is as follows：
In formula, x：y：z=（1-42）：（1-10）：（1-18）.
A kind of high temperature resistant clay stabilizer preparation method of the present invention, comprises the following steps：
1）Will be a certain amount of soluble in water containing sulfonic monomer, with KOH regulation pH value to 6～8；
2）Add epoxychloropropane in reactor, temperature of reactor controls at 10～30 DEG C；
3）Add dimethylamine agueous solution in above-mentioned reactor, contain sulfonic group in unsaturated quaternary ammonium salt and step 1
Monomer solution.Finally being made into monomer gross mass percentage concentration is 30～55%；
4）The logical nitrogen add initiator in above-mentioned reactor, reaction temperature is 40～90 DEG C, the response time is 2～
8h；
5）When step 4 product molecular weight 1500～6000 when, add chain-transferring agent, reaction finishes and obtains
Clay stabilizer.
Wherein, the raw materials used proportioning of described high temperature resistant clay stabilizer：With monomer total amount for 1, the percent mass of each monomer
Than for：Epoxychloropropane 30～60%；Dimethylamine 11～19%, unsaturated quaternary ammonium salt 2～20%, monomer containing sulfonic group 2～20%, first
Sour sodium 0.5%～5%；Finally it is made into the aqueous solution that monomer gross mass percentage concentration is 30%～55%.
Described unsaturated quaternary ammonium salt can be pi-allyl trimethyl ammonium chloride, dimethyl diallyl ammonium chloride, diethyl
One of diallyl ammonium chloride or several mixture.
Described can be 2- acrylamide-2-methylpro panesulfonic acid, vinyl sulfonic acid, acrylamide containing sulfonic monomer
One of butyl sulfonic acid or several mixture.
Described initiator can be water miscible azo-initiator, hydrogen peroxide and ammonium persulfate-sodium bisulfite oxygen
Change reduction system, also can choose potassium peroxydisulfate-sodium sulfite redox system, initiator addition is monomer gross mass
0.1～4.0%；Initiator initiator system of ammonium persulfate-sodium sulfite redox system, sodium sulfite and Ammonium persulfate. mole
Than for 1:1.0～1.3, preferably 1:1.2.
Beneficial effects of the present invention and feature：
（1）The clay stabilizer main chain of the present invention and the equal cation of side chain.The positive charge that main chain contains is more, Ke Yitong
When adsorb with multiple clay particles, formed multipoint adsorption, suppression clay hydration swelling；The nitrogen sun simultaneously containing in side chain
Ion, freedom of movement ratio is larger, disperses migration to have strong control action for clay particle, has very strong water-fast
Washing property.
（2）Containing azochlorosulfonate acid anion on the clay stabilizer side chain of the present invention is strong aquation group, can be in clay
Grain surface forms the hydration shell of densification, can stop and delay hydrone to contact with surface of clay, play and prevent clay aquation swollen
Swollen purpose, also has high temperature resistance, salt resistance, resistant to pollution effect simultaneously.
（3）The clay stabilizer molecular weight of the present invention is low, can be applied to low-permeability oil pool, and consumption is few, effect is good.
Specific embodiment
In order to be better understood from the present invention, it is further elucidated with the content invented with reference to embodiment, but the present invention's is interior
Hold and be not limited only to the following examples.
Embodiment 1
Take 42g 2- acrylamide-2-methylpro panesulfonic acid to be dissolved in 58g water, adjust pH to 7 about with KOH, standby.To
69.4g epoxychloropropane is added, temperature of reactor controls at 20 DEG C, addition 56.3g mass fraction is the two of 40% in reactor
Methylamine water solution and the above-mentioned 2- acrylamide-2-methylpro panesulfonic acid potassium solution having prepared of 50g, are subsequently adding 13.5g alkene
Hydroxypropyltrimonium chloride, 60g water, add the sodium sulfite of 1.1g after being passed through nitrogen 30min in reactor, add after 3min
Enter 2.7g Ammonium persulfate., react 2～8h at temperature is 40 DEG C, detect the molecular weight of product during the course of the reaction, work as molecule
Amount, when 4216, adds 4.1g sodium formate, reaction finishes and obtains a kind of clay stabilizer, as follows through its structural formula of infrared analysiss：
In formula, x：y：z= 5:1:1.
Embodiment 2
Take 40g acrylamide butyl sulfonic acid to be dissolved in 60g water, adjust pH to 7 about with KOH, standby.Add in reactor
Enter 69.4g epoxychloropropane, temperature of reactor controls at 20 DEG C, add the dimethylamine agueous solution that 56.3g mass fraction is 40%
The acrylamide butyl sulfonic acid potassium solution that prepared above-mentioned with 50g, is subsequently adding the dimethyl that 23.4g mass fraction is 70%
Diallyl ammonium chloride aqueous solution, 65g water, add the sodium sulfite of 1.1g after being passed through nitrogen 30min in reactor,
Add 2.7g Ammonium persulfate. after 3min, react 2～8h at temperature is 40 DEG C, detect the molecule of product during the course of the reaction
Amount, when molecular weight is 4330, adds 3.3g sodium formate, reaction finishes and obtains a kind of clay stabilizer, through its knot of infrared analysiss
Structure formula is as follows：
In formula, x：y：z=25:5:6.
Embodiment 3
Take 22g vinyl sulfonic acid to be dissolved in 40g water, adjust pH to 7 about with KOH, standby.Add in reactor
34.7g epoxychloropropane, temperature of reactor controls at 20 DEG C, add 28.2g mass fraction be 40% dimethylamine agueous solution with
The above-mentioned vinyl sulfonic acid potassium solution having prepared of 31g, is subsequently adding the diethyl diallyl that 31.5g mass fraction is 60%
Aqueous ammonium chloride solution, 24 g water, add the sodium sulfite of 0.5g after being passed through nitrogen 30min in reactor, add after 3min
1.3g Ammonium persulfate., reacts 2～8h at temperature is 40 DEG C, detects the molecular weight of product during the course of the reaction, work as molecular weight
When 5517, add 2.5g sodium formate, reaction finishes and obtains a kind of clay stabilizer, as follows through its structural formula of infrared analysiss：
In formula, x：y：z=25:9:10.
Embodiment 4
Weigh 0.5g clay stabilizer sample, add water to 100g, being made into concentration is 0.5% clay stabilization agent solution, wherein viscous
Soil stabilizer structure is
In formula, x：y：z= 5:1:1.
According to China National Petroleum industry standard《Water filling clay stabilizer method of evaluating performance SY/T1994
(2002)》, the preventive effect of expansion of the sample under test room temperature and after 250 DEG C of heat rolling 24h.
Embodiment 5
Weigh 0.5g clay stabilizer sample, add water to 100g, being made into concentration is 0.5% clay stabilization agent solution, wherein viscous
Soil stabilizer structure is
In formula, x：y：z=25:5:6.
According to China National Petroleum industry standard《Water filling clay stabilizer method of evaluating performance SY/T1994
(2002)》, the preventive effect of expansion of the sample under test room temperature and after 250 DEG C of heat rolling 24h.
Embodiment 6
Weigh 0.5g clay stabilizer sample, add water to 100g, being made into concentration is 0.5% clay stabilization agent solution, wherein viscous
Soil stabilizer structure is
In formula, x：y：z=25:9:10.
According to China National Petroleum industry standard《Water filling clay stabilizer method of evaluating performance SY/T1994
(2002)》, the preventive effect of expansion of the sample under test room temperature and after 250 DEG C of heat rolling 24h.
Embodiment 4-6 result of the test is as shown in table 1.
The anti-swollen result of table 1 clay stabilizer
Embodiment 7
Weigh 0.5g clay stabilizer sample, add water to 100g, being made into concentration is 0.5% clay stabilization agent solution, wherein viscous
Soil stabilizer structure is
In formula, x：y：z= 5:1:1.
According to China National Petroleum industry standard《Shale-control agent for drilling fluid evaluation methodology SY/T6335-1997》Enter
The dilatancy test of row sample.Instrument is NP-3 shale expansion tester.
Embodiment 8
Weigh 0.5g clay stabilizer sample, add water to 100g, being made into concentration is 0.5% clay stabilization agent solution, wherein viscous
Soil stabilizer structure is
In formula, x：y：z=25:5:6.
According to China National Petroleum industry standard《Shale-control agent for drilling fluid evaluation methodology SY/T6335-1997》Enter
The dilatancy test of row sample.Instrument is NP-3 shale expansion tester.
Embodiment 9
Weigh 0.5g clay stabilizer sample, add water to 100g, being made into concentration is 0.5% clay stabilization agent solution, wherein viscous
Soil stabilizer structure is
In formula, x：y：z=25:9:10.
According to China National Petroleum industry standard《Shale-control agent for drilling fluid evaluation methodology SY/T6335-1997》Enter
The dilatancy test of row sample.Instrument is NP-3 shale expansion tester.
Embodiment 7-9 result of the test is as shown in table 2.
Table 2 embodiment 7-9 result of the test
| Sample ID | 8h linear expansion rate/% | 16h linear expansion rate/% |
| Embodiment 7 | 51.42 | 68.96 |
| Embodiment 8 | 53.75 | 70.29 |
| Embodiment 9 | 49.31 | 66.38 |
Embodiment 10
Weigh 0.5g clay stabilizer sample, add water to 100g, being made into concentration is 0.5% clay stabilization agent solution, wherein viscous
Soil stabilizer structure is
In formula, x：y：z= 5:1:1.
According to company standard《Q/SH 0053-2010 clay stabilizer technical requirements》At room temperature sample is carried out water-fast
Wash rate performance test.
Embodiment 11
Weigh 0.5g clay stabilizer sample, add water to 100g, being made into concentration is 0.5% clay stabilization agent solution, wherein viscous
Soil stabilizer structure is
In formula, x：y：z=25:5:6.
According to company standard《Q/SH 0053-2010 clay stabilizer technical requirements》At room temperature sample is carried out water-fast
Wash rate performance test.
Embodiment 12
Weigh 0.5g clay stabilizer sample, add water to 100g, being made into concentration is 0.5% clay stabilization agent solution, wherein viscous
Soil stabilizer structure is
In formula, x：y：z=25:9:10.
According to company standard《Q/SH 0053-2010 clay stabilizer technical requirements》At room temperature sample is carried out water-fast
Wash rate performance test.
Embodiment 10-12 result of the test is as shown in table 3
The water-fastness rate of table 3 clay stabilizer
| Sample ID | Bentonite inflated volume (mL) for the first time | Expand bentonite volume (mL) second | Bentonite inflated volume (mL) for the third time | Water-fastness rate (%) |
| Embodiment 10 | 0.89 | 0.90 | 0.90 | 98.89 |
| Embodiment 11 | 0.97 | 0.97 | 0.98 | 98.97 |
| Embodiment 12 | 1.00 | 1.02 | 1.05 | 95.24 |
The above results show, the clay stabilizer of present invention preparation has good heatproof, water-fastness and good suppression
The ability of clay swell processed.
Claims (9)
1. a kind of high temperature resistant clay stabilizer is it is characterised in that this stabilizer is by epoxychloropropane, dimethylamine, unsaturated quaternary ammonium salt
It is polymerized with containing sulfonic monomer, its main chain contains azonia, and its side chain contains azonia and sulfonic acid simultaneously
Root anion；Described clay stabilizer molecular structural formula is as follows：
In formula, x：y：z=（1-42）：（1-14）：（1-10）；Or its molecular structural formula is as follows：
In formula, x：y：z=（1-42）：（1-12）：（1-12）；Or its molecular structural formula is as follows：
In formula, x：y：z=（1-42）：（1-10）：（1-18）.
2. the preparation method of high temperature high efficiency clay stabilizer as claimed in claim 1, it is characterized in that by epoxychloropropane, two
Methylamine, unsaturated quaternary ammonium salt are obtained by the initiation reaction of initiator with containing sulfonic monomer, and lead to during the course of the reaction
Cross addition chain-transferring agent sodium formate and control its molecular weight.
3. as claimed in claim 2 the preparation method of high temperature resistant clay stabilizer it is characterised in that epoxychloropropane is added
To in reactor, temperature control, at 10～30 DEG C, is subsequently adding dimethylamine, unsaturated quaternary ammonium salt, monomer containing sulfonic group, wherein contains
Sulfonic group monomer is previously dissolved in water, adjusts pH to 6～8 with KOH, leads to nitrogen and add initiator, in temperature in reactor
For reacting 2～8h at 40～90 DEG C, when molecular weight is 1500～6000, add chain-transferring agent sodium formate, its addition is single
The 0.5%～5% of body gross mass, reaction finishes and obtains clay stabilizer.
4. as claimed in claim 2 or claim 3 the preparation method of high temperature resistant clay stabilizer it is characterised in that with monomer total amount for 1,
The mass percent of each monomer is：Epoxychloropropane 30～60%；Dimethylamine 11～19%, unsaturated quaternary ammonium salt 2～20%, containing sulphur
Acid-based monomers 2～20%, sodium formate 0.5%～5%；Finally it is made into the aqueous solution that monomer gross mass percentage concentration is 30%～55%.
5. as claimed in claim 2 or claim 3 high temperature resistant clay stabilizer preparation method it is characterised in that：Unsaturated quaternary ammonium salt
For one of pi-allyl trimethyl ammonium chloride, dimethyl diallyl ammonium chloride, diethyl diallyl ammonium chloride or several
The mixture planted.
6. as claimed in claim 2 or claim 3 high temperature resistant clay stabilizer preparation method it is characterised in that：Containing sulfonate radical cloudy from
The monomer of son is one of 2- acrylamide-2-methylpro panesulfonic acid, vinyl sulfonic acid, acrylamide butyl sulfonic acid or several
The mixture planted.
7. as claimed in claim 2 high temperature resistant clay stabilizer preparation method it is characterised in that：Initiator is water miscible
Azo-initiator, hydrogen peroxide, ammonium persulfate-sodium bisulfite redox system or potassium peroxydisulfate-sodium sulfite oxidation
Reduction system, initiator addition is the 0.1～4.0% of monomer gross mass.
8. as claimed in claim 7 high temperature resistant clay stabilizer preparation method it is characterised in that initiator be Ammonium persulfate .-
Sodium sulfite redox system, sodium sulfite and Ammonium persulfate. mol ratio are 1:1.0～1.3.
9. as claimed in claim 8 the preparation method of high temperature resistant clay stabilizer it is characterised in that sodium sulfite and over cure
Sour ammonium mol ratio is 1:1.2.
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| CN106608949B (en) * | 2015-10-26 | 2019-02-22 | 中国石油化工股份有限公司 | A kind of clay stabilizer and preparation method thereof |
| CN105647509A (en) * | 2016-01-21 | 2016-06-08 | 西安石油大学 | Active anti-swelling and swelling-shrinkage agent and preparation method and application thereof |
| CN106753316B (en) * | 2017-02-07 | 2019-10-01 | 西安石油大学 | A kind of multi-functional clay stabilizer |
| CN115404054A (en) * | 2017-07-28 | 2022-11-29 | 克拉玛依市正诚有限公司 | Washing-resistant shrinkage-expansion clay stabilizer and preparation method and application thereof |
| CN108329902A (en) * | 2018-01-23 | 2018-07-27 | 中国石油天然气股份有限公司 | A kind of salt tolerant clay stabilizer and preparation method thereof of oil field water outlet preparing fracturing fluid |
| CN110317586A (en) * | 2018-03-29 | 2019-10-11 | 晋州市茂源钻采技术开发有限公司 | A kind of formula and preparation method thereof of drilling fluid shale potent inhibitor |
| CN111607375B (en) * | 2020-06-16 | 2022-09-23 | 胜利油田凯渡石油技术开发有限公司 | Anti-swelling shrinkage and expansion-shrinkage agent for low-permeability sensitive oil reservoir and preparation method thereof |
| CN114426618B (en) * | 2020-10-14 | 2024-03-22 | 中国石油化工股份有限公司 | Polymer type high-temperature-resistant anti-swelling and shrinking agent and preparation method and application thereof |
| CN114478275B (en) * | 2020-10-27 | 2024-01-16 | 中石化南京化工研究院有限公司 | High-temperature-resistant clay stabilizer and preparation method thereof |
| CN114989799B (en) * | 2022-07-18 | 2022-10-25 | 华巍博大(北京)科技有限公司 | Oligomeric cationic shrinking and swelling agent composition, oligomeric cationic shrinking and swelling agent, and preparation method and application thereof |
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Address after: Liuhe District of Nanjing City, Jiangsu province 210048 geguan Road No. 699 Patentee after: China Petroleum & Chemical Corp. Patentee after: SINOPEC NANJING CHEMICAL RESEARCH INSTITUTE Co.,Ltd. Address before: Liuhe District of Nanjing City, Jiangsu province 210048 geguan Road No. 699 Patentee before: China Petroleum & Chemical Corp. Patentee before: Nanhua Group Research Institute |