CN110105928A - A kind of environment-friendlysticky sticky soil stabilizer of oil field low molecular weight and preparation method thereof - Google Patents
A kind of environment-friendlysticky sticky soil stabilizer of oil field low molecular weight and preparation method thereof Download PDFInfo
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- CN110105928A CN110105928A CN201910380687.9A CN201910380687A CN110105928A CN 110105928 A CN110105928 A CN 110105928A CN 201910380687 A CN201910380687 A CN 201910380687A CN 110105928 A CN110105928 A CN 110105928A
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- 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
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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
- C09K8/60—Compositions for stimulating production by acting on the underground formation
- C09K8/62—Compositions for forming crevices or fractures
- C09K8/66—Compositions based on water or polar solvents
- C09K8/68—Compositions based on water or polar solvents containing organic compounds
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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
- C09K8/60—Compositions for stimulating production by acting on the underground formation
- C09K8/62—Compositions for forming crevices or fractures
- C09K8/72—Eroding chemicals, e.g. acids
- C09K8/74—Eroding chemicals, e.g. acids combined with additives added for specific purposes
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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
- C09K8/60—Compositions for stimulating production by acting on the underground formation
- C09K8/84—Compositions based on water or polar solvents
- C09K8/86—Compositions based on water or polar solvents containing organic compounds
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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
- C09K2208/00—Aspects relating to compositions of drilling or well treatment fluids
- C09K2208/12—Swell inhibition, i.e. using additives to drilling or well treatment fluids for inhibiting clay or shale swelling or disintegrating
Abstract
The invention discloses environment-friendlysticky sticky soil stabilizers of a kind of oil field low molecular weight and preparation method thereof, are compounded by choline chloride and quaternary ammonium salt A mixing；Wherein, mixing quality percentage is choline chloride 60-70%, quaternary ammonium salt A30-40%；The preparation method of quaternary ammonium salt A: firstly, acrylic acid and n-vinyl pyrrolidone are reacted under the action of initiator, intermediate a is obtained；Then, the reaction of intermediate a and N, N- (dialkyl group) ethanol amine, obtains intermediate b；Then, quaternizing agent aqueous solution is added into intermediate b, then adjusts reaction solution system pH to alkalescent, obtains quaternary ammonium salt A.The raw material environmental protection that clay stabilizer of the invention uses is degradable, and low molecular weight is not easy to plug, and stabilizer has both high temperature tolerance and height prevents swollen performance, is suitable for use as preparing the additive of all kinds of underground work liquid such as drilling fluid, fracturing fluid, acid solution, slippery water.
Description
Technical field
The present invention relates to oilfield prospecting developing underground work technical field, in particular to a kind of oil field low molecular weight
Environment-friendlysticky sticky soil stabilizer.
Background technique
Clay mineral mainly has montmorillonite, kaolinite, illite, chlorite, illite/smectite mixed layer, green deceives people several major class such as layer.
Clay mineral widely exists in oil and gas reservoir.These clay mineral grains during the exploration and development in oil field such as drilling well,
Complete well, acidification, pressure break, encounter external water-based fluid in the injecting process after its own will generate expansion or migration, thus meeting
It results in blockage to hole or fracture medium, influences penetrating power and oil gas well production.Generally for the permeability for protecting oil-gas Layer,
It is swollen for the clay of mud shale or loam mould stratum during fracture acidizing transformation or workover treatment to improve oil and gas production
The problems such as swollen, alleviates its expansion or migration using the clay stabilizer of inhibition.
Clay mineral meets stratum permeability injury caused by fresh water expansion Yu gan is moved, and is that one in Petroleum Production seriously asks
Topic.Clay stabilizer can be effectively adsorbed in surface of clay, prevent water sensitivity mineral hydration swelling and dispersion migration and to oil gas
It is injured caused by layer.With the exploitation in oil field, clay stabilizer using more and more extensive, it is required also higher and higher.It wants
Ask clay stabilizer to have the characteristics that washing away for good antiacid liquid, saline solution, lye and grease, and to be suitable for active water,
Perforating fluid, fracturing fluid, drilling fluid and acidifying solution etc. enter well working fluid body.
It is more toxic mostly with phenyl ring in such as poly- ammonium salt of the long steady agent of existing clay or quaternary ammonium salt molecular structure and difficult
With the group of degradation, so that clay stabilizer bio-toxicity with higher.Therefore, the clay stabilizer of non-environmental protection type system
Introducing necessarily brings environmental protection pressure, returns after being discharged to ground, returns drain and has to pass through degradation resolution process, carries out corresponding harmless
Change processing, just will increase the cost of degradation treatment containing the group difficult to degrade such as phenyl ring, so also improve oil-gas field development at
This.In addition, cationic high molecular polymer clay stabilizer easily causes the secondary injury on stratum when being applied in acidization,
Because their molecular weight cross conference blocking stratum, reduce in-place permeability, to reduce the permeability of oily phase.Therefore, it is necessary to
A kind of low molecular weight clay stabilizer with strong rejection capability and the excellent feature of environmental protection is developed, returns being processed into for drain to realize to reduce
This, and reduce the purpose of its pollution to water flooding.
Summary of the invention
It is an object of the present invention to provide a kind of environment-friendlysticky sticky soil stabilizers of oil field low molecular weight.
It is a further object of the present invention to provide a kind of preparation methods of the environment-friendlysticky sticky soil stabilizer of oil field low molecular weight.
The environment-friendlysticky sticky soil stabilizer of oil field low molecular weight provided by the invention by choline chloride and
Quaternary ammonium salt A is compounded.Wherein, mass percent are as follows: choline chloride 60-70% and quaternary ammonium salt A30-
40%.The molecular structural formula of the quaternary ammonium salt A is as follows:
R in formula1And R2It is the chain-like alkyl of carbon atom number between 1 and 3, R3It is chain alkane of the carbon atom number between 2-4
Base.
The quaternary ammonium salt A is by raw material propylene acid, n-vinyl pyrrolidone, N, N- (dialkyl group) ethanol amine, quaternized examination
Agent and initiator for reaction are made；The molecular structural formula of wherein N, N- (dialkyl group) ethanol amine is as follows:
R in formula1And R2It is the chain-like alkyl of carbon atom number between 1 and 3；The molecular structural formula of quaternizing agent are as follows: Cl-
R3, R3It is chain-like alkyl of the carbon atom number between 2-4.The preparation method of quaternary ammonium salt A is comprising steps of step 1, acrylic acid and N-
Vinyl pyrrolidone reacts under the action of initiator, obtains intermediate a；Step 2, intermediate a and N, N- (dialkyl group) second
Hydramine reaction, obtains intermediate b；Step 3, quaternizing agent is added into intermediate b, then adjusts reaction solution system pH to weak
Alkalinity obtains quaternary ammonium salt A.The initiator is ammonium persulfate or sodium hydrogensulfite.
Preferably, the clay stabilizer by mass percent 65% choline chloride and 35% season
Ammonium salt A compounding is made.It is 0.5- that this clay stabilizer, which is applied to the dosage in the underground works liquid such as drilling fluid, fracturing fluid, acid solution,
1wt.%.It is 0.2-0.5wt.% applied to the dosage in slippery water, in the injecting process, additive amount 1-5wt.%.
The preparation method for preparing the environment-friendlysticky sticky soil stabilizer of above-mentioned oil field low molecular weight, specifically comprises the following steps:
S1, quaternary ammonium salt A is prepared, steps are as follows:
S11, distilled water is added into reaction vessel, is passed through nitrogen displacement discharge air；
S12, reaction vessel is added in acrylic acid and n-vinyl pyrrolidone, is stirring evenly and then adding into initiator, heated
Reacting liquid temperature is set to rise to 120 DEG C, constant temperature is stirred to react 30min, obtains intermediate a；
S13, by intermediate a and N, 1:1.05~1.10 is added in reaction vessel N- (dialkyl group) ethanol amine in molar ratio,
Stirring, adds catalyst, is warming up to 110~130 DEG C of reaction 3-6h, obtains intermediate b；
S14, intermediate b is cooled to 80~90 DEG C, quaternizing agent is added in stirring, then uses sodium carbonate or carbonic acid
Hydrogen sodium adjusts reaction solution system pH to 7.5~8.0, reacts 1~2h, obtains quaternary ammonium salt A；
S2, by choline chloride, quaternary ammonium salt A, 60-70%:30-40% is mixed by mass percentage
It stirs evenly to get environment-friendlysticky sticky soil stabilizer is arrived.
In the above method, the catalyst is one kind of butyl titanate, p-methyl benzenesulfonic acid and antimony acetate.
The reaction equation that quaternary ammonium salt A is prepared in step S1 is as follows:
Compared with prior art, the invention has the beneficial effects that:
(1) contain a large amount of quaternary ammonium groups in clay stabilizer of the invention, there is excellent preventive effect of expansion, it is permanent effective,
It is firmly combined with clay, has the advantages that dosage is few, efficiency is high；And molecular weight is small, will not result in blockage.
(2) raw material that the clay stabilizer uses all is low toxicity or nontoxic reagent, without inflammable and explosive or poisonous and hazardous
Reaction raw materials, environmentally protective, reaction condition is mild, safe operation.Choline chloride is as clay stabilizer group
/ mono-, have clay swell inhibiting rate more preferable, anti-dilative is higher.Meanwhile choline chloride belongs to environment-friendly type
Raw material, nontoxic, biodegrade is very fast, is easy degradation treatment, is that a kind of good and environmentally protective clay of preventive effect of expansion is steady
Determine agent；Choline chloride is also a kind of quaternary ammonium salt, is used cooperatively with another quaternary ammonium salt A of the invention, association
Same-action forms the clay stabilizer of compounding.
(3) clay stabilizer is the environment-friendlysticky sticky soil stabilizer that height prevents swollen performance, and it is suitable for various underground work liquid
Body, anti-dilative >=90% have good biocompatibility and the excellent feature of environmental protection, are suitable for use as preparing drilling fluid, pressure break
The additive of all kinds of underground work liquid such as liquid, acid solution, slippery water.
Specific embodiment
Hereinafter, preferred embodiments of the present invention will be described, it should be understood that preferred embodiment described herein is only used
In the description and interpretation present invention, it is not intended to limit the present invention.
Embodiment 1
A kind of preparation method for the environment-friendlysticky sticky soil stabilizer preparing oil field low molecular weight, specifically comprises the following steps:
S1, quaternary ammonium salt A is prepared, steps are as follows:
S11,200 grams of distilled water are added in 500 milliliters of reaction flasks, lead to nitrogen displaced air；
S12, by 7.2g acrylic acid and 11.1gN- vinyl pyrrolidone, (acrylic acid and n-vinyl pyrrolidone are rubbed
You are than 1:1) reaction flask is added, it is stirring evenly and then adding into initiator ammonium persulfate, heating makes reacting liquid temperature rise to 120 DEG C,
Constant temperature is stirred to react 30min, obtains intermediate a；
S13, by intermediate a and N, 1:1.05~1.10 is added in reaction vessel N- (dimethyl) ethanol amine in molar ratio,
Stirring, adds catalyst butyl titanate, is warming up to 110 DEG C of reaction 6h, obtains intermediate b；
S14, intermediate b is cooled to 80 DEG C, quaternizing agent CH is added in stirring3CH2Cl, intermediate b and quaternized examination
The molar ratio of agent is 1:1.5, then adjusts reaction solution system pH to 7.5~8.0 using sodium carbonate or sodium bicarbonate, reaction 1~
2h obtains quaternary ammonium salt A；
S2, choline chloride and quaternary ammonium salt A 3:2 in mass ratio are mixed evenly to get arriving
Environment-friendlysticky sticky soil stabilizer.
Embodiment 2
A kind of preparation method for the environment-friendlysticky sticky soil stabilizer preparing oil field low molecular weight, specifically comprises the following steps:
S1, quaternary ammonium salt A is prepared, steps are as follows:
S11,200 grams of distilled water are added in 500 milliliters of reaction flasks, lead to nitrogen displaced air；
S12, by 7.2g acrylic acid and 12.2gN- vinyl pyrrolidone, (acrylic acid and n-vinyl pyrrolidone are rubbed
You are than 1:1.1) reaction flask is added, it is stirring evenly and then adding into initiator sodium hydrogensulfite, initiator amount (quality) is propylene
3 the percent of acid and n-vinyl pyrrolidone gross mass；Heating makes reacting liquid temperature rise to 120 DEG C, and constant temperature is stirred to react
30min obtains intermediate a；
S13, by intermediate a and N, 1:1.05~1.10 is added in reaction vessel N- (diethyl) ethanol amine in molar ratio,
Stirring, adds catalyst p-methyl benzenesulfonic acid, and catalyst amount (quality) is intermediate a and N, the total matter of N- (diethyl) ethanol amine
2 the percent of amount, are warming up to 120 DEG C of reaction 5h, obtain intermediate b；
S14, intermediate b is cooled to 90 DEG C, quaternizing agent CH is added in stirring3CH2CH2Cl, intermediate b with it is quaternized
The molar ratio of reagent is 1:1.5, then adjusts reaction solution system pH to 7.5~8.0 using sodium bicarbonate, reacts 1~2h, obtains
Quaternary ammonium salt A；
S2, by choline chloride and quaternary ammonium salt A 65:35 in mass ratio be mixed evenly to get
To environment-friendlysticky sticky soil stabilizer.
Embodiment 3
A kind of preparation method for the environment-friendlysticky sticky soil stabilizer preparing oil field low molecular weight, specifically comprises the following steps:
S1, quaternary ammonium salt A is prepared, steps are as follows:
S11,200 grams of distilled water are added in 500 milliliters of reaction flasks, lead to nitrogen displaced air；
S12, reaction flask is added in acrylic acid and n-vinyl pyrrolidone that molar ratio is 1.1:1, after mixing evenly
Initiator sodium hydrogensulfite is added, heating makes reacting liquid temperature rise to 120 DEG C, and constant temperature is stirred to react 30min, obtains intermediate a；
S13, by intermediate a and N, 1:1.05~1.10 is added in reaction vessel N- (dipropyl) ethanol amine in molar ratio,
Stirring, adds catalyst acetic acid antimony, is warming up to 130 DEG C of reaction 4h, obtains intermediate b；
S14, intermediate b is cooled to 90 DEG C, quaternizing agent CH is added in stirring3CH2CH2CH2Then Cl uses carbonic acid
Hydrogen sodium adjusts reaction solution system pH to 7.5~8.0, reacts 1~2h, obtains quaternary ammonium salt A；
S2, by choline chloride and quaternary ammonium salt A according to mass ratio 7:3 be mixed evenly to get
To environment-friendlysticky sticky soil stabilizer.
Performance test:
Hereinafter the clay stabilizer of Examples 1 to 3 preparation is carried out preventing swollen performance.
Since dosage of the environment-friendlysticky sticky soil stabilizer in all kinds of underground work liquid such as drilling fluid, fracturing fluid, acid solution is
0.5-1wt.%.Dosage in slippery water is 0.2-0.5wt.%.Therefore only it is formulated as in following henchnmrk test
The solution of 0.2~1wt.% prevents that swollen performance is evaluated.
According to SY/T 5971-2016 anti-dilative detection method as standard, its anti-dilative is surveyed using centrifugal process
Examination, i.e., by measuring in bentonite in powder respectively in the environment-friendlysticky sticky soil stabilizer of addition 0.2wt.%, 0.5wt.% and 1wt.%
Afterwards, by measuring the volume expansion increment of bentonite in powder, to prevent that swollen performance is evaluated to the clay stabilizer；Wherein, real
Testing test temperature is 150 DEG C.
In this experiment, the calculation formula of anti-dilative are as follows:In formula, B is anti-clayswelling rate, %；
V0The volume for being bentonite in kerosene, mL；V1For volume of the bentonite in clay stabilization agent solution, mL；V2Exist for bentonite
Volume in water, mL.
Test result is as follows shown in table 1 for the anti-dilative of the clay stabilizer of Examples 1 to 3 preparation.
The anti-dilative test data of table 1, clay stabilizer under the conditions of various concentration
From the experimental result in table 1 it is found that at a temperature of bentonite of the clay stabilizer of Examples 1 to 3 preparation at 150 DEG C
Anti-dilative reach 90% or more, illustrate that the clay stabilizer of the application shows excellent to prevent swollen performance.
In addition, after clay stabilizer prepared by Examples 1 to 3 is placed 30 days, 50 days, 100 days respectively, using above-mentioned phase
It is detected with method and prevents swollen performance, and test experiments result is consistent substantially with the test result in upper table 1, at 150 DEG C
At a temperature of bentonitic anti-dilative still can achieve 90% or more, it is seen that clay stabilizer disclosed in the present application prevents swollen performance
Duration was more than 1 month.
Cytotoxic evaluation is carried out to the environment-friendlysticky sticky soil stabilizer of Examples 1 to 3 preparation below.
The specific steps of Cytotoxic evaluation (MTT cell experiment) experimental method are as follows: S1, cell kind plate: by logarithmic growth
Phase is cells trypsinised, is configured to cell suspension, is inoculated in 96 orifice plates by 3000~5000 cell per wells, every hole adds
100uL is placed in CO2(5%) overnight incubation is adherent at 37 DEG C in incubator, and edge hole is filled with sterile PBS；S2, institute in table 2 is pressed
The mass fraction preparation program shown carries out agent-feeding treatment (experimental drug is clay stabilizer), and each concentration of specimens carries out 3~5
It repeats to test；S3, MTT reaction: being separately added into 20 μ L MTT solution (5mg/ml, i.e. 0.5%MTT) in all holes, in incubator
It is incubated for 4 hours；S4, DMSO Rong Xie formazan；Careful to absorb supernatant: every hole adds 150 μ L of DMSO (dimethyl sulfoxide), low in shaking table
Fast (120~140rpm/min) concussion 10min dissolves crystal sufficiently；S5, it surveys absorbance value: being measured using microplate reader
Clay stabilizer is calculated as follows to the appreciation rate or survival rate of cell in 490nm absorbance value；Wherein, experimental period is
72h.In this experiment, the calculation formula of proliferation rate or survival rate A (%) are as follows:In formula, A1For experiment
The absorbance value of group cell DMSO dissolution, A2For the absorbance value of cellular control unit DMSO dissolution, A0For the absorbance of DMSO solution
Value.The cytotoxicity test data of the clay stabilizer prepared in Examples 1 to 3 are as shown in table 2 below.
The cell survival rate of table 2, clay stabilizer under the conditions of various concentration
The method for recommending to evaluate cytotoxicity classification referring to standard GB/T/T16175-2008, cell proliferation rate >=
It is 0 grade when 100%, is 1 grade when 80~99%, 0 grade and 1 grade of toxic reaction are qualification.Therefore, from the test result in table 2
It is found that the cell survival rate of the clay stabilizer of different experiments concentration is fallen in 113~126% section, that is, illustrate that clay is steady
Determine agent and does not show apparent cytotoxicity.
In conclusion clay stabilizer prepared by the embodiment of the present invention 1~3 has both high temperature tolerance and height prevents swollen property and good
Good biocompatibility.
The above described is only a preferred embodiment of the present invention, be not intended to limit the present invention in any form, though
So the present invention has been disclosed as a preferred embodiment, and however, it is not intended to limit the invention, any technology people for being familiar with this profession
Member, without departing from the scope of the present invention, when the technology contents using the disclosure above make a little change or modification
For the equivalent embodiment of equivalent variations, but anything that does not depart from the technical scheme of the invention content, according to the technical essence of the invention
Any simple modification, equivalent change and modification to the above embodiments, all of which are still within the scope of the technical scheme of the invention.
Claims (9)
1. a kind of environment-friendlysticky sticky soil stabilizer of oil field low molecular weight, which is characterized in that by choline chloride
It is compounded with quaternary ammonium salt A；The molecular structural formula of the quaternary ammonium salt A is as follows:
R in formula1And R2It is the chain-like alkyl of carbon atom number between 1 and 3, R3It is chain-like alkyl of the carbon atom number between 2-4.
2. the environment-friendlysticky sticky soil stabilizer of oil field low molecular weight as described in claim 1, which is characterized in that the matter of each component
It is as follows to measure percentage: choline chloride 60-70% and quaternary ammonium salt A30-40%.
3. the environment-friendlysticky sticky soil stabilizer of oil field low molecular weight as claimed in claim 2, which is characterized in that the quaternary ammonium salt
A is by raw material propylene acid, n-vinyl pyrrolidone, N, N- (dialkyl group) ethanol amine, quaternizing agent and initiator for reaction system
At；The molecular structural formula of wherein N, N- (dialkyl group) ethanol amine is as follows:
R in formula1And R2It is the chain-like alkyl of carbon atom number between 1 and 3；The molecular structural formula of quaternizing agent are as follows: Cl-R3, R3It is
Chain-like alkyl of the carbon atom number between 2-4.
4. the environment-friendlysticky sticky soil stabilizer of oil field low molecular weight as claimed in claim 3, which is characterized in that the quaternary ammonium salt A
Preparation method comprising steps of step 1, acrylic acid and n-vinyl pyrrolidone are reacted under the action of initiator, obtain
Mesosome a；Step 2, the reaction of intermediate a and N, N- (dialkyl group) ethanol amine, obtains intermediate b；Step 3, it is added into intermediate b
Then quaternizing agent adjusts reaction solution system pH to alkalescent, obtains quaternary ammonium salt A.
5. the environment-friendlysticky sticky soil stabilizer of oil field low molecular weight as claimed in claim 4, which is characterized in that the initiator
For ammonium persulfate or sodium hydrogensulfite.
6. the environment-friendlysticky sticky soil stabilizer of oil field low molecular weight as claimed in claim 5, which is characterized in that the clay stabilization
Agent is compounded and is made by the choline chloride of mass percent 65% and 35% quaternary ammonium salt A.
7. the environment-friendlysticky sticky soil stabilizer of oil field low molecular weight as claimed in claim 6, which is characterized in that the clay stabilization
Agent is 0.5-1wt.% applied to the dosage in drilling fluid, fracturing fluid, acid solution, the dosage 0.2-0.5wt.% in slippery water,
In the injecting process, additive amount 1-5wt.%.
8. a kind of preparation method of the clay stabilizer as described in claim 1-7 any one, which is characterized in that including as follows
Step:
S1, quaternary ammonium salt A is prepared, steps are as follows:
S11, distilled water is added into reaction vessel, is passed through nitrogen displacement discharge air；
S12, reaction vessel is added in acrylic acid and n-vinyl pyrrolidone, is stirring evenly and then adding into initiator, heating makes anti-
Liquid temperature is answered to rise to 120 DEG C, constant temperature is stirred to react 30min, obtains intermediate a；
S13, by intermediate a and N, 1:1.05~1.10 is added in reaction vessel N- (dialkyl group) ethanol amine in molar ratio, stirring,
Catalyst is added, 110~130 DEG C of reaction 3-6h is warming up to, obtains intermediate b；
S14, intermediate b is cooled to 80~90 DEG C, quaternizing agent is added in stirring, then uses sodium carbonate or sodium bicarbonate
Reaction solution system pH to 7.5~8.0 is adjusted, 1~2h is reacted, obtains quaternary ammonium salt A；
S2, by choline chloride, quaternary ammonium salt A, 60-70%:30-40% is mixed by mass percentage
Uniformly to get arrive environment-friendlysticky sticky soil stabilizer.
9. the preparation method of environment-friendlysticky sticky soil stabilizer as claimed in claim 8, which is characterized in that the catalyst is metatitanic acid
One kind of four butyl esters, p-methyl benzenesulfonic acid and antimony acetate.
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| CN110564230A (en) * | 2019-07-26 | 2019-12-13 | 四川羽玺新材料股份有限公司 | Environment-friendly nano composite material coating |
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