CN106590580A - Salinity resistant foam scrubbing agent composition used for drainage gas recovery and preparation method and application thereof - Google Patents
Salinity resistant foam scrubbing agent composition used for drainage gas recovery and preparation method and application thereof Download PDFInfo
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Abstract
The invention relates to a salinity resistant foam scrubbing agent composition used for drainage gas recovery and a preparation method and application thereof. The salinity resistant foam scrubbing agent composition used for drainage gas recovery aims at solving the problems of reduction of output and even flowing stop of gas wells caused by excessive hydrops during developing of the current gas wells. According to the adopted technical scheme, the foam scrubbing agent is prepared from, by mole fraction, 1 part of long chain polyether nitrogen compound and 0.5-20 parts of sulfonated fatty acid alkyl ester, wherein the general molecular formula of the long chain polyether nitrogen compound is shown as a formula (I), and R1 is a fatty group of C8-C30; y is a PO chain segment adding number; z is a EO chain segment adding number; R2 is a alkylene of C1-C4; R3, R4 are any one of a alkyl group and a substituted alkyl group; the salinity resistant foam scrubbing agent composition used for drainage gas recovery solves the problem well. The foaming height of the salinity resistant foam scrubbing agent composition is larger than 200 mm, the liquid carrying capability of the hypersalinity resistant foam scrubbing agent composition is larger than 140 mL, and the salinity resistant foam scrubbing agent composition can be used for the drainage gas recovery of hyperhaline gas wells. . The formula is shown in the description.
Description
Technical field
The present invention relates to a kind of anti-salinity water pumping gas production foam discharging agent composition and preparation method and application, belongs to oil
Gas field chemical agent technical field.
Background technology
With the reinforcement of gas-field exploitation dynamics, the key issue that gas field water outlet is normally produced into restriction gas well.Foaming water discharge
Gas production is a kind of drainage gas recovery that recent domestic is developed rapidly, with equipment is simple, easy construction, low cost,
Applicable well depth scope is big, the advantages of do not affect gas well normally to produce.So-called foaming water discharge is exactly by the mineralized water of shaft bottom
Introduce some surfactants with specific function so as to during gas-liquid two-phase mixing perpendicular flow, produce a large amount of
Low-density resistance aqueous foam, foam takes water with air-flow from shaft bottom to ground, improves gas-liquid and vertically lifts liquid energy power, reaches draining and adopts
The purpose of gas.When gas field temperature and salinity are raised, the foamability and stability of foam discharging agent are all greatly reduced, usually
The effect of water pumping gas production is not reached.Therefore need exploitation that there is resisting high temperature, high salt, the foam discharging agent of height foaming efficiency.
At present water pumping gas production foaming agent adopts Recompounded multielement system mostly, at the same comprising nonionic surface active agent and from
Subtype surfactant.In order to strengthen the stability of single foam, alkali, alcohol, polymer, alkane are generally additionally added in formula
The auxiliary agents such as alkylolamides form strengthening foam.Patent CN102212344A discloses a kind of high-temperature foam scrubbing agent for drainage gas recovery,
Its component is by mass fraction:10~15 parts of lauryl sodium sulfate, 2~5 parts of APG, AES15~18 part, ten
20~25 parts of dialkyl sulfonates, 5~10 parts of biosurfactant, 27~48 parts of water, its salt resistant character is poor.Specially
Sharp CN102212348A discloses a kind of salt tolerant, methanol tolerance foam discharging agent, and individual component content by weight percentage is:Cocounut oil
Amido propyl betaine 20~40%, amine oxide 45~65%, alpha-alkene sulfonate 5~20%, triethanolamine 5~15%,
Fluorocarbon surfactant 0.2~2%, methyl alcohol 0~5%, can be resistant to salinity up to 180,000, but the agent contains fluorocarbon surface
Activating agent, not only cost greatly improve and have greater environmental impacts.
The content of the invention
One of the technical problem to be solved is that on stream hydrops is excessive for existing gas well, causes gas well to subtract
Produce the problem of even stop-spraying, there is provided a kind of gas well foam discharging agent composition for efficiently taking liquid, with good salt resistant character, rise
Bubble performance and fluid-carrying capability.
The two of the technical problem to be solved use for the anti-salinity water pumping gas production for solving one of above-mentioned technical problem
The preparation method of foam discharging agent composition.
The three of the technical problem to be solved arrange to provide a kind of anti-salinity for solving one of above-mentioned technical problem
The hydromining gas application process of foam discharging agent composition.
To solve one of above-mentioned technical problem, the technical solution used in the present invention is as follows:A kind of anti-salinity water pumping gas production is used
Foam discharging agent composition includes following components with molar fraction:
(1) 1 part of long-chain polyether nitrogen-containing compound;
(2) 0.5~20 parts of aliphatic acid sulfoalkyl acid amides;
Described long-chain polyether nitrogen-containing compound has following general molecular formula:
Wherein, R1For C8~C30Fat-based;Y adds sum, y=0~20 for PO segments;Z adds sum for EO segments,
Z=0~60;R2For C1~C4Alkylidene;R3、R4For C1~C5Alkyl, replace alkyl in any one.
In above-mentioned technical proposal, the R1For C8~C30Fat-based, acyl group, carbonyl, ether, hydroxyl can be contained
Can be saturated carbon chains Deng group, it is also possible to containing unsaturated carbon chains, as preferred R1Preferred version be C10~C20
Alkyl, alkylbenzene.
In above-mentioned technical proposal, the R2Preferably C2H4Or C3H6, more preferably C2H4。
In above-mentioned technical proposal, the R3、R4For C1~C5Alkyl, replace alkyl in any one;Wherein institute
State and replace the substituent in alkyl to be the substituted radicals such as hydroxyl substituent, halogenic substituent.
In above-mentioned technical proposal, the preferred version of the z is more than 0, more preferably less than equal to 30, further preferably
For z=1~20.
In above-mentioned technical proposal, the preferred version of the y is more preferably y=1~20 more than 0.
In above-mentioned technical proposal, the aliphatic acid sulfoalkyl acid amides preferably has general molecular formula shown in formula (II):
R in formula (II)5For C5~C30Fat-based, R6For C1~C4Alkylidene or substituted alkylene;M is to make formula (II)
Shown molecule is in electroneutral cation, and j is the number of M, and the value of j is the inverse of M valence state values.
In above-mentioned technical proposal, when M is preferably+1 valency, the aliphatic acid sulfoalkyl acid amides has shown in formula (III)
General molecular formula:
M preferably is selected from any one metal ion or ammonium ion in alkali metal;Further preferably:M preferred versions are alkali gold
Any one metal ion in category, more preferably sodium or potassium ion, more preferably scheme are selected from sodium ion;
R5Preferred version is selected from C8~C22Alkyl, more preferably scheme is selected from C10~C16Alkyl;R6Preferred version is
Selected from C1~C2Alkylidene.
In above-mentioned technical proposal, long-chain polyether nitrogen-containing compound is 1 with the mol ratio of aliphatic acid sulfoalkyl acid amides:
(0.2~10).
Foaming agent combination in the present invention does not have particular/special requirement when preparing to water, can be deionized water, can be with
It is the water containing inorganic mineral, and the water for containing inorganic mineral can be running water, gas well stratum water or gas well injection water.
To solve the two of above-mentioned technical problem, the technical solution used in the present invention is as follows:Anti- salinity water pumping gas production is arranged with bubble
The preparation method of agent composition, comprises the following steps:
(1) synthesis of long-chain polyether nitrogen-containing compound
A, in the presence of base catalyst, R1OH obtains R with aequum propylene oxide reaction1O(CHCH3CH2O)yH;
B, in the presence of base catalyst, R1O(CHCH3CH2O)yH is obtained with aequum reacting ethylene oxide
R1O(CHCH3CH2O)y(CH2CH2O)z+1H;
C, by R1O(CHCH3CH2O)y(CH2CH2O)z+1H reacts Jing after processing with thionyl chloride and obtains
R1O(CHCH3CH2O)y(CH2CH2O)zR2Cl;
D, by R1O(CHCH3CH2O)y(CH2CH2O)z R2Cl and NR3R4In a solvent, reaction temperature 70~
90 DEG C of reactions obtain R Jing after processing1O(CHCH3CH2O)y(CH2CH2O)z R2NR3R4;
E, by R1O(CHCH3CH2O)y(CH2CH2O)z R2NR3R4With hydrogen peroxide in 60~70 DEG C of reactions, Jing process
After obtain long-chain polyether nitrogen-containing compound;
(2) preparation of foam discharging agent composition
The desired amount of long-chain polyether nitrogen-containing compound, aliphatic acid sulfoalkyl acid amides are well mixed and must resist salinity water pumping gas production
Use foam discharging agent composition.
The key active ingredient of foam discharging agent of the present invention is aliphatic acid sulfoalkyl acid amides and long-chain polyether nitrogen-containing compound, this area
Technical staff knows, for the ease of transport and store or onsite application etc. from the aspect of, various supply forms can be adopted,
Such as water-free solid-state form, or aqueous solid-state form, or aqueous cream form, or aqueous solution form;
Aqueous solution form includes being made into the form of concentrate with water, is directly made into the foam discharging agent form of live desired concn;Wherein,
There is no particular/special requirement to water, can be deionized water, can also be the water containing inorganic mineral, and contain inorganic mineral
Water can be running water, gas well stratum water or gas well injection water.
In order to solve the three of technical problem, the technical solution used in the present invention is:The arbitrary described anti-ore deposit of above-mentioned technical proposal
The change degree water pumping gas production application of foam discharging agent composition.
In above-mentioned technical proposal, the application, those skilled in the art can be according to related process of the prior art by institute
In the anti-salinity water pumping gas production foam discharging agent composition application stated and gas well water pumping gas production, the stratum water of gas well is preferably suitable for
Salinity is 0~250000mg/L.
In the long-chain polyether nitrogen-containing compound of the anti-salinity water pumping gas production foam discharging agent of the present invention comprising EO, PO etc. it is non-from
Sub-piece, can dramatically increase the salt resistant character of foam discharging agent, while it is a kind of amine oxide, be affected less by pH value,
Into nonionic surfactant under neutral or alkalescence, cationic is shown under acid condition, be a kind of multifunction surface activity
Agent, with stronger foam enhancing foam stability energy, has synergy well with anion surfactant;Aliphatic acid sulfoalkyl acid amides
With good foaming and foam stabilizing ability, and there is preferable salt-resistance, both form compounding synergy after mixing, strengthen
The fluid-carrying capability and foam stability energy of foam.
The foam discharging agent composition of the present invention is applicable to gas well of the salinity less than 250000mg/L.According to SY/T
6465-2000《Foam drainage gas recovery foaming agent evaluation method》Foaming properties test is carried out to the foam discharging agent, foaming is high
Degree is more than 200mm, and liquid carry over is more than 140mL, with good frothing capacity, foam stability and fluid-carrying capability,
Achieve preferable technique effect.
In order to be better understood from the present invention, present disclosure is expanded on further with reference to embodiments, but the present invention's is interior
Appearance is not limited solely to the following examples.
Specific embodiment
【Embodiment 1】
The preparation of composition CX-1, preparation process:
(1) long-chain polyether nitrogen-containing compound (C12H25O(CHCH3CH2O)3(CH2CH2O)7CH2CH2N(CH3)2O)
Synthesis with prepare:
186.0 grams of dodecanols, 5.6 grams of potassium hydroxide are added in the pressure reactor equipped with agitating device, is heated to
When 80~90 DEG C, vacuum system is opened, be dehydrated under a high vacuum 1 hour, then with nitrogen displacement 3~4 times, by body
It is that reaction temperature is adjusted to 150 DEG C and is slowly passed through 179.9 grams of expoxy propane, control pressure≤0.60MPa is cooled to 90 DEG C,
Low-boiling-point substance is removed in vacuum, system reaction temperature is adjusted to 150 DEG C and is slowly passed through 360.0 grams of oxirane, control pressure by continuation
Power≤0.60MPa.After reaction terminates, neutralization, dehydration, obtain C after cooling12H25O(CHCH3CH2O)3(CH2CH2O)8
H, yield 98.8wt%.
339 are added in the four round flask equipped with reflux condensate device, thermometer, agitator and gas absorbing device
Gram C12H25O(CHCH3CH2O)3(CH2CH2O)8H and 57 gram of pyridine, is heated to 70 DEG C under stirring, use dropping funel
85 grams of thionyl chlorides are slowly added dropwise, are reacted 10 hours at 90 DEG C after completion of dropping.After reaction terminates, reactant is stood,
Cooling layering, neutrality is neutralized to sodium hydroxide solution by upper strata, with saturated common salt water washing 5-6 time of heat, after drying
Obtain intermediate product C12H25O(CHCH3CH2O)3(CH2CH2O)7CH2CH2Cl, yield is 88%.
By C12H25O(CHCH3CH2O)3(CH2CH2O)7CH2CH2143 grams of Cl add with reflux condensate device,
In thermometer, the four-hole boiling flask of agitator, 77 DEG C are heated to, by N (CH3)2Solution dropping funel slowly drips to flask
In, system remains alkalescent, stratification after reacting 10 hours.By the saturation food after the vacuum distillation of upper strata with heat
Salt water washing 5-6 time, obtains desired intermediate C12H25O(CHCH3CH2O)3(CH2CH2O)7
CH2CH2N(CH3)2, yield is 83%.
By C12H25O(CHCH3CH2O)3(CH2CH2O)7CH2CH2N(CH3)2100 grams are added to returned cold
In solidifying device, thermometer, the four-hole boiling flask of agitator, 60 DEG C are heated to, are slowly added dropwise H2O230 grams of solution,
React 5 hours at 70 DEG C, with petroleum ether extraction, vacuum drying, analyze by high performance liquid chromatography (HPLC), produce
C in thing12H25O(CHCH3CH2O)3(CH2CH2O)7CH2CH2N(CH3)2O content is 97.72wt%.
(2) preparation of foaming agent combination:
At normal temperatures and pressures, 70 grams of long-chain polyether nitrogen-containing compound obtained by synthesis is weighed in previous step in reactor,
Add appropriate local originally water dissolves;63.6 grams of aliphatic acid sulfoalkyl acid amides are added thereto to again, are added enough
Local running water is configured to the solution of 30wt% to 445 grams, is sufficiently stirred for 30min to being completely dissolved, obtains final product
Foaming agent combination CX-1.
【Embodiment 2】
The preparation of composition CX-2, preparation process:
(1) long-chain polyether nitrogen-containing compound (C16H33O(CHCH3CH2O)10(CH2CH2O)20CH2CH2
N(C2H5)(C3H7O) O) synthesis with prepare:
121 grams of hexadecanols, 3 grams of potassium hydroxide are added in the pressure reactor equipped with agitating device, it is heated to 80~
When 90 DEG C, vacuum system is opened, be dehydrated under a high vacuum 1 hour, it is then with nitrogen displacement 3~4 times, system is anti-
Answer temperature to be adjusted to 150 DEG C and be slowly passed through 300 grams of expoxy propane, control pressure≤0.60MPa is cooled to 90 DEG C, vacuum
Low-boiling-point substance is removed, system reaction temperature is adjusted to 150 DEG C and is slowly passed through 500.0 grams of oxirane, control pressure by continuation
≤0.60MPa.After reaction terminates, neutralization, dehydration, obtain C after cooling16H33O(CHCH3CH2O)10(CH2CH2O)21H,
Yield 98.6wt%.
131 are added in the four round flask equipped with reflux condensate device, thermometer, agitator and gas absorbing device
Gram C16H33O(CHCH3CH2O)10(CH2CH2O)21H and 20 gram of pyridine, is heated to 70 DEG C under stirring, use dropping funel
35 grams of thionyl chlorides are slowly added dropwise, are reacted 10 hours at 90 DEG C after completion of dropping.After reaction terminates, reactant is stood,
Cooling layering, neutrality is neutralized to sodium hydroxide solution by upper strata, with saturated common salt water washing 5-6 time of heat, after drying
Obtain intermediate product C16H33O(CHCH3CH2O)10(CH2CH2O)20CH2CH2Cl, yield is 86.6%.
By C16H33O(CHCH3CH2O)10(CH2CH2O)20CH2CH2135 grams of Cl add with reflux condensate device,
In thermometer, the four-hole boiling flask of agitator, 77 DEG C are heated to, by N (C2H5)(C3H6OH) solution is slow with dropping funel
In dripping to flask, system remains alkalescent, stratification after reacting 10 hours.Heat will be used after the vacuum distillation of upper strata
Saturated common salt water washing 5-6 time, obtain desired intermediate C16H33O(CHCH3CH2O)10(CH2CH2O)20
CH2CH2N(C2H5)(C3H7O), yield is 83.3%.
By C16H33O(CHCH3CH2O)10(CH2CH2O)20CH2CH2N(C2H5)(C3H7O) 100 grams are added to band
In having the four-hole boiling flask of reflux condensate device, thermometer, agitator, 60 DEG C are heated to, are slowly added dropwise H2O2Solution 30
Gram, react 5 hours at 70 DEG C, with petroleum ether extraction, vacuum drying, Jing high performance liquid chromatography (HPLC) is analyzed,
C in product16H33O(CHCH3CH2O)10(CH2CH2O)20CH2CH2N(C2H5)(C3H7O) O content is 96.32
Wt%.
(2) preparation of foaming agent combination:
At normal temperatures and pressures, 50 grams of long-chain polyether nitrogen-containing compound obtained by synthesis is weighed in previous step in reactor,
Add appropriate local originally water dissolves;81.5 grams of aliphatic acid sulfoalkyl acid amides is added thereto to again, is added enough
Local running water to 438 grams, be configured to the solution of 30wt%, be sufficiently stirred for 30min to being completely dissolved, i.e.,
Obtain foaming agent combination CX-2.
【Embodiment 3】
The preparation of composition CX-3, preparation process:
(1) long-chain polyether nitrogen-containing compound (C14H29OC3H6O(CH2CH2O)8CH2CH2N(C3H7O)2O conjunction)
Into with preparation:
107.0 grams of tetradecanols, 3.0 grams of potassium hydroxide are added in the pressure reactor equipped with agitating device, is heated to
When 80~90 DEG C, vacuum system is opened, be dehydrated under a high vacuum 1 hour, then with nitrogen displacement 3~4 times, by body
It is that reaction temperature is adjusted to 150 DEG C and is slowly passed through 60 grams of expoxy propane, control pressure≤0.60MPa is cooled to 90 DEG C, very
Sky removes low-boiling-point substance, and system reaction temperature is adjusted to 150 DEG C and is slowly passed through 203.0 grams of oxirane, control pressure by continuation
≤0.60MPa.After reaction terminates, neutralization, dehydration, obtain C after cooling14H29OCHCH3CH2O(CH2CH2O)9H,
Yield 98.7wt%.
327 are added in the four round flask equipped with reflux condensate device, thermometer, agitator and gas absorbing device
Gram C14H29OCHCH3CH2O(CH2CH2O)9H and 20 gram of pyridine, is heated to 70 DEG C under stirring, slow with dropping funel
35 grams of thionyl chlorides are added dropwise, are reacted 10 hours at 90 DEG C after completion of dropping.Reaction terminate after, by reactant stand, it is cold
But it is layered, upper strata is neutralized to into neutrality with sodium hydroxide solution, with saturated common salt water washing 5-6 time of heat, must after being dried
To intermediate product C14H29OCHCH3CH2O(CH2CH2O)8CH2CH2Cl, yield is 87%.
By C14H29OCHCH3CH2O(CH2CH2O)8CH2CH2165 grams of Cl is added and is carried reflux condensate device, temperature
In degree meter, the four-hole boiling flask of agitator, 77 DEG C are heated to, by N (C3H6OH)2Solution dropping funel slowly drips to burning
In bottle, system remains alkalescent, stratification after reacting 10 hours.The saturation of heat will be used after the vacuum distillation of upper strata
Brine It 5-6 time, obtains desired intermediate C14H29OCHCH3CH2O(CH2CH2O)8CH2CH2N(C3H7
O)2, yield is 83.3%.
By C14H29OCHCH3CH2O(CH2CH2O)8CH2CH2N(C3H7O)2100 grams are added to reflux condensation mode
In device, thermometer, the four-hole boiling flask of agitator, 60 DEG C are heated to, are slowly added dropwise H2O230 grams of solution, at 70 DEG C
Lower reaction 5 hours, with petroleum ether extraction, vacuum drying, Jing high performance liquid chromatography (HPLC) analysis, in product
C14H29OCHCH3CH2O(CH2CH2O)8CH2CH2N(C3H7O)2O content is 96.71wt%.
(2) preparation of foaming agent combination:
At normal temperatures and pressures, 90 grams of long-chain polyether nitrogen-containing compound obtained by synthesis is weighed in previous step in reactor,
Add appropriate local originally water dissolves;7.7 grams of aliphatic acid sulfoalkyl acid amides is added thereto to again, is added enough
Local running water is configured to the solution of 30wt% to 327 grams, is sufficiently stirred for 30min to being completely dissolved, obtains final product
Foaming agent combination CX-3.
【Embodiment 4】
The preparation of composition CX-4, preparation process:
(1) long-chain polyether nitrogen-containing compound (C20H33O(C3H6O)5(CH2CH2O)3CH2CH2N(C3H7)(C5H11)O)
Synthesis with prepare:
145.0 grams of myristyl phenol, 2.0 grams of potassium hydroxide are added in the pressure reactor equipped with agitating device, plus
When heat is to 80~90 DEG C, vacuum system is opened, be dehydrated under a high vacuum 1 hour, then with nitrogen displacement 3~4 times,
System reaction temperature is adjusted to into 150 DEG C and is slowly passed through 300 grams of expoxy propane, control pressure≤0.60MPa is cooled to 90 DEG C,
Low-boiling-point substance is removed in vacuum, system reaction temperature is adjusted to 150 DEG C and is slowly passed through 180.0 grams of oxirane, control pressure by continuation
Power≤0.60MPa.After reaction terminates, neutralization, dehydration, obtain C after cooling20H33O(C3H6O)5(CH2CH2O)4H, receives
Rate 99.6wt%.
218 are added in the four round flask equipped with reflux condensate device, thermometer, agitator and gas absorbing device
Gram C20H33O(C3H6O)5(CH2CH2O)4H and 20 gram of pyridine, is heated to 70 DEG C under stirring, be slowly added dropwise with dropping funel
35 grams of thionyl chlorides, react 10 hours after completion of dropping at 90 DEG C.After reaction terminates, reactant is stood, cooling divides
Layer, neutrality is neutralized to sodium hydroxide solution by upper strata, with saturated common salt water washing 5-6 time of heat, in obtaining after drying
Between product C20H33O(C3H6O)5(CH2CH2O)3CH2CH2Cl, yield is 87.1%.
By C20H33O(C3H6O)5(CH2CH2O)3CH2CH296 grams of Cl add with reflux condensate device, thermometer,
In the four-hole boiling flask of agitator, 77 DEG C are heated to, by N (C3H7)(C5H11) solution dropping funel slowly drips to flask
In, system remains alkalescent, stratification after reacting 10 hours.By the saturation food after the vacuum distillation of upper strata with heat
Salt water washing 5-6 time, obtains desired intermediate C20H33O(C3H6O)5(CH2CH2O)3CH2CH2N(C3H7)(C5H1 1), yield is 83.7%.
By C20H33O(C3H6O)5(CH2CH2O)3CH2CH2N(C3H7)(C5H11) 100 grams be added to reflux condensation mode
In device, thermometer, the four-hole boiling flask of agitator, 60 DEG C are heated to, are slowly added dropwise H2O230 grams of solution, at 70 DEG C
Lower reaction 5 hours, with petroleum ether extraction, vacuum drying, Jing high performance liquid chromatography (HPLC) analysis, in product
C20H33O(C3H6O)5(CH2CH2O)3CH2CH2N(C3H7)(C5H11) O content be 97.61wt%.
(2) preparation of foaming agent combination:
At normal temperatures and pressures, 90 grams of long-chain polyether nitrogen-containing compound obtained by synthesis is weighed in previous step in reactor,
Add appropriate local originally water dissolves;32.1 grams of aliphatic acid sulfoalkyl acid amides is added thereto to again, is added enough
Local running water to 407 grams, be configured to the solution of 30wt%, be sufficiently stirred for 30min to being completely dissolved, i.e.,
Obtain foaming agent combination CX-4.
【Embodiment 5】
The preparation of composition CX-5, preparation process:
(1) long-chain polyether nitrogen-containing compound (C12H25O(CHCH3CH2O)20(CH2CH2O)15CH2CH2N(CH3)(C2H5)
O synthesis) and preparation:
93.0 grams of dodecanols, 5.6 grams of potassium hydroxide are added in the pressure reactor equipped with agitating device, it is heated to 80~
When 90 DEG C, vacuum system is opened, be dehydrated under a high vacuum 1 hour, it is then with nitrogen displacement 3~4 times, system is anti-
Answer temperature to be adjusted to 150 DEG C and be slowly passed through 600 grams of expoxy propane, control pressure≤0.60MPa is cooled to 90 DEG C, vacuum
Low-boiling-point substance is removed, system reaction temperature is adjusted to 150 DEG C and is slowly passed through 720 grams of oxirane, control pressure by continuation
≤0.60MPa.After reaction terminates, neutralization, dehydration, obtain C after cooling12H25O(CHCH3CH2O)20(CH2CH2O)16H,
Yield 98.6wt%.
287 are added in the four round flask equipped with reflux condensate device, thermometer, agitator and gas absorbing device
Gram C12H25O(CHCH3CH2O)20(CH2CH2O)16H and 30 gram of pyridine, is heated to 70 DEG C under stirring, use dropping funel
35 grams of thionyl chlorides are slowly added dropwise, are reacted 10 hours at 90 DEG C after completion of dropping.After reaction terminates, reactant is stood,
Cooling layering, neutrality is neutralized to sodium hydroxide solution by upper strata, with saturated common salt water washing 5-6 time of heat, after drying
Obtain intermediate product C12H25O(CHCH3CH2O)20(CH2CH2O)15CH2CH2Cl, yield is 88%.
By C12H25O(CHCH3CH2O)20(CH2CH2O)15CH2CH2146 grams of Cl add with reflux condensate device,
In thermometer, the four-hole boiling flask of agitator, 77 DEG C are heated to, by N (CH3)(C2H5) solution dropping funel slowly drips
To in flask, system remains alkalescent, stratification after reacting 10 hours.Heat will be used after the vacuum distillation of upper strata
Saturated common salt water washing 5-6 time, obtains desired intermediate C12H25O(CHCH3CH2O)20(CH2CH2O)15CH2CH2
N(CH3)(C2H5), yield is 83.3%.
By C12H25O(CHCH3CH2O)20(CH2CH2O)15CH2CH2N(CH3)(C2H5) 100 grams be added to and carry back
In stream condensing unit, thermometer, the four-hole boiling flask of agitator, 60 DEG C are heated to, are slowly added dropwise H2O230 grams of solution,
React 5 hours at 70 DEG C, with petroleum ether extraction, vacuum drying, Jing high performance liquid chromatography (HPLC) analysis, produce
C in thing12H25O(CHCH3CH2O)20(CH2CH2O)15CH2CH2N(CH3)(C2H5) O content be 96.97wt%.
(2) preparation of foaming agent combination:
At normal temperatures and pressures, 90 grams of long-chain polyether nitrogen-containing compound obtained by synthesis is weighed in previous step in reactor,
Add appropriate local originally water dissolves;8.5 grams of aliphatic acid sulfoalkyl acid amides is added thereto to again, is added enough
Local running water is configured to the solution of 30wt% to 328 grams, is sufficiently stirred for 30min to being completely dissolved, obtains final product
Foaming agent combination CX-5.
【Embodiment 6】
The preparation of composition CX-6, preparation process:
(1) long-chain polyether nitrogen-containing compound (C12H25O(CHCH3CH2O)15(CH2CH2O)10CH2CH2
N(CH3)2O synthesis) and preparation:
93.0 grams of dodecanols, 5.6 grams of potassium hydroxide are added in the pressure reactor equipped with agitating device, it is heated to 80~
When 90 DEG C, vacuum system is opened, be dehydrated under a high vacuum 1 hour, it is then with nitrogen displacement 3~4 times, system is anti-
Answer temperature to be adjusted to 150 DEG C and be slowly passed through 450 grams of expoxy propane, control pressure≤0.60MPa is cooled to 90 DEG C, vacuum
Low-boiling-point substance is removed, system reaction temperature is adjusted to 150 DEG C and is slowly passed through 495 grams of oxirane, control pressure by continuation
≤0.60MPa.After reaction terminates, neutralization, dehydration, obtain C after cooling12H25O(CHCH3CH2O)15(CH2CH2O)11H,
Yield 98.6wt%.
269 are added in the four round flask equipped with reflux condensate device, thermometer, agitator and gas absorbing device
Gram C12H25O(CHCH3CH2O)15(CH2CH2O)11H and 57 gram of pyridine, is heated to 70 DEG C under stirring, use dropping funel
85 grams of thionyl chlorides are slowly added dropwise, are reacted 10 hours at 90 DEG C after completion of dropping.After reaction terminates, reactant is stood,
Cooling layering, neutrality is neutralized to sodium hydroxide solution by upper strata, with saturated common salt water washing 5-6 time of heat, after drying
Obtain intermediate product C12H25O(CHCH3CH2O)15(CH2CH2O)10CH2CH2Cl, yield is 88.3%.
By C12H25O(CHCH3CH2O)15(CH2CH2O)10CH2CH2115 grams of Cl add with reflux condensate device,
In thermometer, the four-hole boiling flask of agitator, 77 DEG C are heated to, by N (CH3)2Solution dropping funel slowly drips to flask
In, system remains alkalescent, stratification after reacting 10 hours.By the saturation food after the vacuum distillation of upper strata with heat
Salt water washing 5-6 time, obtains desired intermediate C12H25O(CHCH3CH2O)15(CH2CH2O)10CH2CH2N(CH3)2, yield is 83.8%.
By C12H25O(CHCH3CH2O)15(CH2CH2O)10CH2CH2N(CH3)2100 grams are added to returned cold
In solidifying device, thermometer, the four-hole boiling flask of agitator, 60 DEG C are heated to, are slowly added dropwise H2O230 grams of solution,
React 5 hours at 70 DEG C, with petroleum ether extraction, vacuum drying, Jing high performance liquid chromatography (HPLC) analysis, product
Middle C12H25O(CHCH3CH2O)15(CH2CH2O)10CH2CH2N(CH3)2O content is 97.32wt%.
(2) preparation of foaming agent combination:
At normal temperatures and pressures, 40 grams of long-chain polyether nitrogen-containing compound obtained by synthesis is weighed in previous step in reactor,
Add appropriate local originally water dissolves;53.9 grams of aliphatic acid sulfoalkyl acid amides is added thereto to again, is added enough
Local running water to 312 grams, be configured to the solution of 30wt%, be sufficiently stirred for 30min to being completely dissolved, i.e.,
Obtain foaming agent combination CX-6.
【Embodiment 7】
The preparation of composition CX-7, preparation process:
(1) long-chain polyether nitrogen-containing compound (C12H25O(CHCH3CH2O)8CH2CH2OCH2CH2N(CH3)2O)
Synthesis with prepare:
93.0 grams of dodecanols, 5.6 grams of potassium hydroxide are added in the pressure reactor equipped with agitating device, it is heated to 80~
When 90 DEG C, vacuum system is opened, be dehydrated under a high vacuum 1 hour, it is then with nitrogen displacement 3~4 times, system is anti-
Answer temperature to be adjusted to 150 DEG C and be slowly passed through 240 grams of expoxy propane, control pressure≤0.60MPa is cooled to 90 DEG C, vacuum
Low-boiling-point substance is removed, system reaction temperature is adjusted to 150 DEG C and is slowly passed through 90 grams of oxirane, control pressure by continuation
≤0.60MPa.After reaction terminates, neutralization, dehydration, obtain C after cooling12H25O(CHCH3CH2O)8(CH2CH2O)2H,
Yield 98.6wt%.
269 are added in the four round flask equipped with reflux condensate device, thermometer, agitator and gas absorbing device
Gram C12H25O(CHCH3CH2O)8(CH2CH2O)2H and 57 gram of pyridine, is heated to 70 DEG C under stirring, slow with dropping funel
Slowly 85 grams of thionyl chlorides are added dropwise, are reacted 10 hours at 90 DEG C after completion of dropping.After reaction terminates, reactant is stood,
Cooling layering, neutrality is neutralized to sodium hydroxide solution by upper strata, with saturated common salt water washing 5-6 time of heat, after drying
Obtain intermediate product C12H25O(CHCH3CH2O)8CH2CH2O CH2CH2Cl, yield is 88.3%.
By C12H25O(CHCH3CH2O)8CH2CH2OCH2CH2115 grams of Cl is added and is carried reflux condensate device, temperature
In meter, the four-hole boiling flask of agitator, 77 DEG C are heated to, by N (CH3)2Solution dropping funel is slowly dripped in flask,
System remains alkalescent, stratification after reacting 10 hours.The saturated aqueous common salt of heat will be used after the vacuum distillation of upper strata
Washing 5-6 time, obtains desired intermediate C12H25O(CHCH3CH2O)8CH2CH2OCH2CH2N(CH3)2, receive
Rate is 83.8%.
By C12H25O(CHCH3CH2O)8CH2CH2OCH2CH2N(CH3)2100 grams are added to reflux condensation mode dress
Put, in the four-hole boiling flask of thermometer, agitator, be heated to 60 DEG C, be slowly added dropwise H2O230 grams of solution, at 70 DEG C
Lower reaction 5 hours, with petroleum ether extraction, vacuum drying, Jing high performance liquid chromatography (HPLC) analysis, in product
C12H25O(CHCH3CH2O)8CH2CH2OCH2CH2N(CH3)2O content is 97.32wt%.
(2) preparation of foaming agent combination:
At normal temperatures and pressures, 40 grams of long-chain polyether nitrogen-containing compound obtained by synthesis is weighed in previous step in reactor,
Add appropriate local originally water dissolves;84.3 grams of aliphatic acid sulfoalkyl acid amides is added thereto to again, is added enough
Local running water to 414 grams, be configured to the solution of 30wt%, be sufficiently stirred for 30min to being completely dissolved, i.e.,
Obtain foaming agent combination CX-7.
【Embodiment 8】
The preparation of composition CX-8, preparation process:
(1) long-chain polyether nitrogen-containing compound (C14H21O(CHCH3CH2O)6(CH2CH2O)12CH2CH2N(CH3)2O)
Synthesis with prepare:
103.0 grams of octyl phenols, 5.6 grams of potassium hydroxide are added in the pressure reactor equipped with agitating device, is heated to
When 80~90 DEG C, vacuum system is opened, be dehydrated under a high vacuum 1 hour, then with nitrogen displacement 3~4 times, by body
It is that reaction temperature is adjusted to 150 DEG C and is slowly passed through 174 grams of expoxy propane, control pressure≤0.60MPa is cooled to 90 DEG C,
Low-boiling-point substance is removed in vacuum, system reaction temperature is adjusted to 150 DEG C and is slowly passed through 286 grams of oxirane, control pressure by continuation
≤0.60MPa.After reaction terminates, neutralization, dehydration, obtain C after cooling14H21O(CHCH3CH2O)6(CH2CH2O)13H,
Yield 98.6wt%.
269 are added in the four round flask equipped with reflux condensate device, thermometer, agitator and gas absorbing device
Gram C14H21O(CHCH3CH2O)6(CH2CH2O)13H and 57 gram of pyridine, is heated to 70 DEG C under stirring, use dropping funel
85 grams of thionyl chlorides are slowly added dropwise, are reacted 10 hours at 90 DEG C after completion of dropping.After reaction terminates, reactant is stood,
Cooling layering, neutrality is neutralized to sodium hydroxide solution by upper strata, with saturated common salt water washing 5-6 time of heat, after drying
Obtain intermediate product C14H21O(CHCH3CH2O)6(CH2CH2O)12CH2CH2Cl, yield is 88.3%.
By C14H21O(CHCH3CH2O)6(CH2CH2O)12CH2CH2115 grams of Cl add with reflux condensate device,
In thermometer, the four-hole boiling flask of agitator, 77 DEG C are heated to, by N (CH3)2Solution dropping funel slowly drips to flask
In, system remains alkalescent, stratification after reacting 10 hours.By the saturation food after the vacuum distillation of upper strata with heat
Salt water washing 5-6 time, obtains desired intermediate C14H21O(CHCH3CH2O)6(CH2CH2O)12CH2CH2N(CH3)2, yield is 83.8%.
By C14H21O(CHCH3CH2O)6(CH2CH2O)12CH2CH2N(CH3)2100 grams are added to reflux condensation mode
In device, thermometer, the four-hole boiling flask of agitator, 60 DEG C are heated to, are slowly added dropwise H2O230 grams of solution, at 70 DEG C
Lower reaction 5 hours, with petroleum ether extraction, vacuum drying, Jing high performance liquid chromatography (HPLC) analysis, in product
C14H21O(CHCH3CH2O)6(CH2CH2O)12CH2CH2N(CH3)2O content is 97.32wt%.
(2) preparation of foaming agent combination:
At normal temperatures and pressures, 40 grams of long-chain polyether nitrogen-containing compound obtained by synthesis is weighed in previous step in reactor,
Add appropriate local originally water dissolves;97.7 grams of aliphatic acid sulfoalkyl acid amides is added thereto to again, is added enough
Local running water to 459 grams, be configured to the solution of 30wt%, be sufficiently stirred for 30min to being completely dissolved, i.e.,
Obtain foaming agent combination CX-8.
【Embodiment 9】
The preparation of composition CX-9, preparation process:
(1) long-chain polyether nitrogen-containing compound (C10H21O(CHCH3CH2O)3(CH2CH2O)7CH2CH2N(CH3)2O)
Synthesis with prepare:
172.0 grams of decane alcohol, 5.6 grams of potassium hydroxide are added in the pressure reactor equipped with agitating device, it is heated to 80~
When 90 DEG C, vacuum system is opened, be dehydrated under a high vacuum 1 hour, it is then with nitrogen displacement 3~4 times, system is anti-
Answer temperature to be adjusted to 150 DEG C and be slowly passed through 179.9 grams of expoxy propane, control pressure≤0.60MPa is cooled to 90 DEG C, very
Sky removes low-boiling-point substance, and system reaction temperature is adjusted to 150 DEG C and is slowly passed through 360.0 grams of oxirane, control pressure by continuation
≤0.60MPa.After reaction terminates, neutralization, dehydration, obtain C after cooling10H21O(CHCH3CH2O)3(CH2CH2O)8H,
Yield 98.7wt%.
325 are added in the four round flask equipped with reflux condensate device, thermometer, agitator and gas absorbing device
Gram C10H21O(CHCH3CH2O)3(CH2CH2O)8H and 57 gram of pyridine, is heated to 70 DEG C under stirring, slow with dropping funel
Slowly 85 grams of thionyl chlorides are added dropwise, are reacted 10 hours at 90 DEG C after completion of dropping.After reaction terminates, reactant is stood,
Cooling layering, neutrality is neutralized to sodium hydroxide solution by upper strata, with saturated common salt water washing 5-6 time of heat, after drying
Obtain intermediate product C10H21O(CHCH3CH2O)3(CH2CH2O)7CH2CH2Cl, yield is 88.1%.
By C10H21O(CHCH3CH2O)3(CH2CH2O)7CH2CH2137 grams of Cl is added and is carried reflux condensate device, temperature
In degree meter, the four-hole boiling flask of agitator, 77 DEG C are heated to, by N (CH3)2Solution dropping funel is slowly dripped in flask,
System remains alkalescent, stratification after reacting 10 hours.The saturated aqueous common salt of heat will be used after the vacuum distillation of upper strata
Washing 5-6 time, obtains desired intermediate C10H21O(CHCH3CH2O)3(CH2CH2O)7CH2CH2N(CH3)2,
Yield is 83.7%.
By C10H21O(CHCH3CH2O)3(CH2CH2O)7CH2CH2N(CH3)2100 grams are added to reflux condensation mode
In device, thermometer, the four-hole boiling flask of agitator, 60 DEG C are heated to, are slowly added dropwise H2O230 grams of solution, at 70 DEG C
Lower reaction 5 hours, with petroleum ether extraction, vacuum drying, Jing high performance liquid chromatography (HPLC) analysis, in product
C10H21O(CHCH3CH2O)3(CH2CH2O)7CH2CH2N(CH3)2O content is 97.33wt%.
(2) preparation of foaming agent combination:
At normal temperatures and pressures, 40 grams of long-chain polyether nitrogen-containing compound obtained by synthesis is weighed in previous step in reactor,
Add appropriate local originally water dissolves;40.8 grams of aliphatic acid sulfoalkyl acid amides is added thereto to again, is added enough
Local running water to 269 grams, be configured to the solution of 30wt%, be sufficiently stirred for 30min to being completely dissolved, i.e.,
Obtain foaming agent combination CX-9.
【Embodiment 10】
Prepare salinity and be respectively 80000mg/L, the simulation water of 150000mg/L, 200000mg/L, with reference to SY/T
6450-2000《Foam drainage gas recovery foaming agent evaluation method》Standard, determines foaming power, the foam stabilization of foam discharging agent
The performances such as property, fluid-carrying capability.The results are shown in Table shown in 2.
The foam discharging agent component structure of table 1
Foaming agent | R1 | y | z | R2 | R3 | R4 | R5 | R6 | I and II mol ratio |
CX-1 | C12H25 | 3 | 7 | C2H4 | CH3 | CH3 | C12H25 | C2H4 | 1:2 |
CX-2 | C16H33 | 10 | 20 | C2H4 | C2H5 | C3H7O | C10H21 | CH2 | 1:10 |
CX-3 | C14H29 | 1 | 8 | C2H4 | C3H7O | C3H7O | C12H25 | C2H4 | 1:0.2 |
CX-4 | C20H33 | 5 | 3 | C2H4 | C3H7 | C5H11 | C10H21 | C2H4 | 1:1 |
CX-5 | C12H25 | 20 | 15 | C2H4 | C2H5 | CH3 | C16H33 | C2H4 | 1:0.5 |
CX-6 | C12H25 | 15 | 10 | C2H4 | CH3 | CH3 | C18H37 | C2H4 | 1:5 |
CX-7 | C12H25 | 8 | 1 | C2H4 | CH3 | CH3 | C12H25 | CH2 | 1:5 |
CX-8 | C14H21 | 6 | 12 | C2H4 | CH3 | CH3 | C14H29 | CH2 | 1:8 |
CX-9 | C10H21 | 3 | 7 | C2H4 | CH3 | CH3 | C14H29 | C2H4 | 1:2 |
The foaming properties of the foam discharging agent composition in the embodiment of table 2
【Comparative example 1】
Use【Embodiment 1】The C of middle synthesis12H25O(CHCH3CH2O)3(CH2CH2O)7CH2CH2N(CH3)2O,
【Embodiment 2】The C of middle synthesis16H33O(CHCH3CH2O)10(CH2CH2O)20CH2CH2N(C2H5)(C3H7O) O,
【Embodiment 3】The C of middle synthesis14H29OC3H6O(CH2CH2O)8CH2CH2N(C3H7O)2O,【Embodiment 4】In
The C of synthesis20H33O(C3H6O)5(CH2CH2O)3CH2CH2N(C3H7)(C5H11) O single dose, be added without subsequent component
Foaming agent combination is prepared into, together【Embodiment 10】Foaming properties test is carried out, be the results are shown in Table shown in 3.
【Comparative example 2】
C is used respectively12H25CONHCH2SO3Na, C14H29CONHCH2SO3Na, C18H37CONHC2H4SO3Na
Single dose, together【Embodiment 10】Foaming properties test is carried out, be the results are shown in Table shown in 3.
【Comparative example 3】
At normal temperatures and pressures, weigh 70 grams of DDAO in reactor, add it is appropriate it is local from
Carry out water dissolves;69 grams of C are added thereto to again12H25CONHC2H4SO3Na, adds enough local running water to 463
Gram, the solution of 30wt% is configured to, 30min is sufficiently stirred for being completely dissolved, foaming agent combination CX-10 is obtained final product,
Together【Embodiment 10】Foaming properties test is carried out, as a result to be shown in Table 3.
The foaming properties of the foam discharging agent single dose in the comparative example of table 3
Claims (9)
1. a kind of anti-salinity water pumping gas production foam discharging agent composition, in terms of molfraction, including following components:
(1) 1 part of long-chain polyether nitrogen-containing compound;
(2) 0.5~20 parts of aliphatic acid sulfoalkyl acid amides;
Described long-chain polyether nitrogen-containing compound has general molecular formula shown in formula (I):
In formula (I), R1For C8~C30Fat-based;Y adds sum, y=0~20 for PO segments;Z adds sum, z=0~60 for EO segments;R2For C1~C4Alkylidene;R3、R4For C1~C5Alkyl, replace alkyl in any one.
2. anti-salinity water pumping gas production foam discharging agent composition according to claim 1, it is characterised in that the R1For C10~C20Alkyl, alkylbenzene at least one.
3. anti-salinity water pumping gas production foam discharging agent composition according to claim 1, it is characterised in that the R2For C2H4Or C3H6。
4. anti-salinity water pumping gas production foam discharging agent composition according to claim 1, it is characterised in that y=1~20;Z=1~30.
5. anti-salinity water pumping gas production foam discharging agent composition according to claim 1, it is characterised in that described aliphatic acid sulfoalkyl acid amides has general molecular formula shown in formula (II):
R in formula (II)5For C5~C30Fat-based, R6For C1~C4Alkylidene or substituted alkylene;To make molecule shown in formula (II) in electroneutral cation, j is the number of M to M, and the value of j is the inverse of M valence state values.
6. anti-salinity water pumping gas production foam discharging agent composition according to claim 1, it is characterised in that the long-chain polyether nitrogen-containing compound is 1 with the mol ratio of aliphatic acid sulfoalkyl acid amides:(0.2~10).
7. the arbitrary described anti-salinity water pumping gas production preparation method of foam discharging agent composition of claim 1~6, comprises the following steps:
(1) synthesis of long-chain polyether nitrogen-containing compound
A, in the presence of base catalyst, R1OH obtains R with aequum propylene oxide reaction1O(CHCH3CH2O)yH;
B, in the presence of base catalyst, R1O(CHCH3CH2O)yH obtains R with aequum reacting ethylene oxide1O(CHCH3CH2O)y(CH2CH2O)z+1H;
C, by R1O(CHCH3CH2O)y(CH2CH2O)z+1H reacts with thionyl chloride and obtains R Jing after processing1O(CHCH3CH2O)y(CH2CH2O)zR2Cl;
D, by R1O(CHCH3CH2O)y(CH2CH2O)zR2Cl and NR3R4In a solvent, R is obtained Jing after processing in 70~90 DEG C of reactions of reaction temperature1O(CHCH3CH2O)y(CH2CH2O)zR2NR3R4;
E, by R1O(CHCH3CH2O)y(CH2CH2O)zR2NR3R4With hydrogen peroxide in 60~70 DEG C of reactions, Jing after processing long-chain polyether nitrogen-containing compound is obtained;
(2) preparation of foam discharging agent composition
The desired amount of long-chain polyether nitrogen-containing compound, aliphatic acid sulfoalkyl acid amides are well mixed must resist salinity water pumping gas production foam discharging agent composition.
8. claim 1~6 arbitrary described anti-salinity water pumping gas production application of foam discharging agent composition.
9. the anti-salinity water pumping gas production according to claim 8 application of foam discharging agent composition, it is characterised in that the formation water salinity for being suitable for gas well is 0~250000mg/L.
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CN109679605B (en) * | 2017-10-18 | 2021-07-30 | 中国石油化工股份有限公司 | Solid foam drainage agent composition, preparation method and application |
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