CN106590574A - Hypersalinity resistant foam scrubbing agent composition used for drainage gas recovery and preparation method and application thereof - Google Patents
Hypersalinity resistant foam scrubbing agent composition used for drainage gas recovery and preparation method and application thereof Download PDFInfo
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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
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- C09K8/00—Compositions for drilling of boreholes or wells; Compositions for treating boreholes or wells, e.g. for completion or for remedial operations
- C09K8/58—Compositions for enhanced recovery methods for obtaining hydrocarbons, i.e. for improving the mobility of the oil, e.g. displacing fluids
- C09K8/584—Compositions for enhanced recovery methods for obtaining hydrocarbons, i.e. for improving the mobility of the oil, e.g. displacing fluids characterised by the use of specific surfactants
Abstract
The invention relates to a hypersalinity resistant foam scrubbing agent composition used for drainage gas recovery and a preparation method and application thereof. The hypersalinity 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 hypersalinity resistant foam scrubbing agent composition used for drainage gas recovery solves the problem well. The foaming height of the hypersalinity 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 hypersalinity 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-high salinity water pumping gas production foam discharging agent compositionss and preparation method and application, belong 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 foam adopts Recompounded multielement system mostly, at the same comprising nonionic surfactant 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 sodium lauryl sulphate, 2～5 parts of alkyl polyglucoside, 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：Cocos nucifera oil
Amido propyl betaine 20～40%, amine oxide 45～65%, alpha-alkene sulfonate 5～20%, triethanolamine 5～15%,
Fluorocarbon surfactant 0.2～2%, methanol 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 compositionss 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 are the anti-high salinity water pumping gas production for solving one of above-mentioned technical problem
With the preparation method of foam discharging agent compositionss.
The three of the technical problem to be solved are a kind of anti-high salinity for solving one of above-mentioned technical problem of offer
The water pumping gas production application process of foam discharging agent compositionss.
To solve one of above-mentioned technical problem, the technical solution used in the present invention is as follows：A kind of anti-high salinity water pumping gas production
Following components is included with molar fraction with foam discharging agent compositionss：
(1) 1 part of long-chain polyether nitrogen-containing compound；
(2) 0.5～20 parts of fatty acid sulfoalkyl ester；
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 group 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 fatty acid sulfoalkyl ester 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) molecule shown in 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 fatty acid sulfoalkyl ester has shown point of formula (III)
Sub- formula：
M preferably is selected from any one metal ion or ammonium ion in alkali metal；Further preferably：M preferred versions are alkali
Any one metal ion in metal, 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 choosing
From C1～C2Alkylidene.
In above-mentioned technical proposal, long-chain polyether nitrogen-containing compound is 1 with the mol ratio of fatty acid sulfoalkyl ester:(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 tap 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- high salinity water pumping gas production bubble
The preparation method of row's agent compositionss, 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)zR2Cl and NR3R4In a solvent, reaction temperature 70～
90 DEG C of reactions obtain R Jing after processing1O(CHCH3CH2O)y(CH2CH2O)zR2NR3R4；
E, by R1O(CHCH3CH2O)y(CH2CH2O)zR2NR3R4With 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 compositionss
The desired amount of long-chain polyether nitrogen-containing compound, fatty acid sulfoalkyl ester mix homogeneously must be resisted into high salinity water pumping gas production
Use foam discharging agent compositionss.
The key active ingredient of foam discharging agent of the present invention is fatty acid sulfoalkyl ester and long-chain polyether nitrogen-containing compound, this area skill
Art personnel know, for the ease of transport and store or onsite application etc. from the aspect of, various supply forms, example 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 concentrated solution 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 tap 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-height of above-mentioned technical proposal
The salinity water pumping gas production application of foam discharging agent compositionss.
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-high salinity water pumping gas production foam discharging agent compositionss application stated and gas well water pumping gas production, the stratum of gas well is preferably suitable for
Water salinity is 0～250000mg/L.
It is non-comprising EO, PO etc. in the long-chain polyether nitrogen-containing compound of the anti-high salinity water pumping gas production foam discharging agent of the present invention
Ion fragment, can dramatically increase the salt resistant character of foam discharging agent, while it is a kind of amine oxide, by pH value affected compared with
It is little, into nonionic surfactant under neutral or alkalescence, cationic is shown under acid condition, it is a kind of multifunction surface
Activating agent, with stronger foam enhancing foam stability energy, has good synergism with anion surfactant；Fatty acid sulfoalkyl
Ester has good foam stabilizing ability, and has preferable salt-resistance, and both form compounding synergism after mixing, strengthen foam
Fluid-carrying capability and foam stability energy.
The foam discharging agent compositionss of the present invention are applicable to gas well of the salinity less than 250000mg/L.According to SY/T
6465-2000《Foam drainage gas recovery foaming agent evaluation methodology》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 compositionss 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 funnel
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 funnel slowly drips to flask
In, system remains alkalescence, 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 dissolution；60.8 grams of fatty acid sulfoalkyl esters are added thereto to again, add enough sheets
Ground tap water is configured to the solution of 30wt% to 436 grams, is sufficiently stirred for 30min to being completely dissolved, obtains final product bubble
Foam agent compositionss CX-1.
【Embodiment 2】
The preparation of compositionss 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 funnel
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 funnel
In dripping to flask, system remains alkalescence, 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 dissolution；77.4 grams of fatty acid sulfoalkyl ester is added thereto to again, is added enough
Local tap water is configured to the solution of 30wt% to 424 grams, is sufficiently stirred for 30min to being completely dissolved, obtains final product
Foaming agent combination CX-2.
【Embodiment 3】
The preparation of compositionss 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 funnel
35 grams of thionyl chlorides of Deca, react 10 hours after completion of dropping at 90 DEG C.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 funnel slowly drips to burning
In bottle, system remains alkalescence, 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 dissolution；7.4 grams of fatty acid sulfoalkyl ester is added thereto to again, adds enough sheets
Ground tap water is configured to the solution of 30wt% to 324 grams, is sufficiently stirred for 30min to being completely dissolved, obtains final product bubble
Foam agent compositionss CX-3.
【Embodiment 4】
The preparation of compositionss 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 funnel
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 funnel slowly drips to flask
In, system remains alkalescence, 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 dissolution；30.5 grams of fatty acid sulfoalkyl ester is added thereto to again, is added enough
Local tap water is configured to the solution of 30wt% to 401 grams, is sufficiently stirred for 30min to being completely dissolved, obtains final product
Foaming agent combination CX-4.
【Embodiment 5】
The preparation of compositionss 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 funnel
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 funnel slowly drips
To in flask, system remains alkalescence, 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 units, 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 dissolution；8.2 grams of fatty acid sulfoalkyl ester is added thereto to again, adds enough sheets
Ground tap water is configured to the solution of 30wt% to 327 grams, is sufficiently stirred for 30min to being completely dissolved, obtains final product bubble
Foam agent compositionss CX-5.
【Embodiment 6】
The preparation of compositionss 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 funnel
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 funnel slowly drips to flask
In, system remains alkalescence, 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 dissolution；52 grams of fatty acid sulfoalkyl ester is added thereto to again, adds enough sheets
Ground tap water is configured to the solution of 30wt% to 306 grams, is sufficiently stirred for 30min to being completely dissolved, obtains final product bubble
Foam agent compositionss CX-6.
【Embodiment 7】
The preparation of compositionss 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 funnel
85 grams of thionyl chlorides of slow Deca, react 10 hours after completion of dropping at 90 DEG C.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 funnel is slowly dripped in flask,
System remains alkalescence, 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 dissolution；80.4 grams of fatty acid sulfoalkyl ester is added thereto to again, is added enough
Local tap water is configured to the solution of 30wt% to 401 grams, is sufficiently stirred for 30min to being completely dissolved, obtains final product
Foaming agent combination CX-7.
【Embodiment 8】
The preparation of compositionss 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 funnel
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 funnel slowly drips to flask
In, system remains alkalescence, 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 dissolution；93.6 grams of fatty acid sulfoalkyl ester is added thereto to again, is added enough
Local tap 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-8.
【Embodiment 9】
The preparation of compositionss 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 funnel
85 grams of thionyl chlorides of slow Deca, react 10 hours after completion of dropping at 90 DEG C.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 funnel is slowly dripped in flask,
System remains alkalescence, 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 dissolution；39.2 grams of fatty acid sulfoalkyl ester is added thereto to again, is added enough
Local tap water is configured to the solution of 30wt% to 264 grams, is sufficiently stirred for 30min to being completely dissolved, obtains final product
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 methodology》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
| Foam | 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 compositionss 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 respectively12H25COOCH2SO3Na, C14H29COOCH2SO3Na, C18H37COOC2H4SO3Na single doses,
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 20 grams of dimethyl dodecyl amine oxide in reactor, add it is appropriate it is local from
Carry out water dissolution；57.3 grams of C are added thereto to again12H25COOC2H4SO3Na, adds enough local tap waters to 258
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-high salinity water pumping gas production foam discharging agent compositionss, in terms of molfraction, including with the following group
Point：
(1) 1 part of long-chain polyether nitrogen-containing compound；
(2) 0.5～20 parts of fatty acid sulfoalkyl ester；
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 is EO segments
Plus sum, z=0～60；R2For C1～C4Alkylidene；R3、R4For C1～C5Alkyl, replace alkyl in
Any one.
2. anti-high salinity water pumping gas production foam discharging agent compositionss according to claim 1, its feature exists
In the R1For C10～C20Alkyl, alkylbenzene at least one.
3. anti-high salinity water pumping gas production foam discharging agent compositionss according to claim 1, its feature exists
In the R2For C2H4Or C3H6。
4. anti-high salinity water pumping gas production foam discharging agent compositionss according to claim 1, its feature exists
In y=1～20；Z=1～30.
5. anti-high salinity water pumping gas production foam discharging agent compositionss according to claim 1, its feature exists
There is general molecular formula shown in formula (II) in described fatty acid sulfoalkyl ester：
R in formula (II)5For C5～C30Fat-based, R6For C1～C4Alkylidene or substituted alkylene；M
To make molecule shown in formula (II) in electroneutral cation, j is the number of M, and the value of j is M valence state values
It is reciprocal.
6. anti-high salinity water pumping gas production foam discharging agent compositionss according to claim 1, its feature exists
In the mol ratio of the long-chain polyether nitrogen-containing compound and fatty acid sulfoalkyl ester be 1:(0.2～10).
7. claim 1～6 arbitrary described anti-high salinity water pumping gas production preparation side of foam discharging agent compositionss
Method, 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)zR2Cl and NR3R4In a solvent, in reaction temperature
70～90 DEG C of reactions obtain R Jing after processing1O(CHCH3CH2O)y(CH2CH2O)zR2NR3R4；
E, by R1O(CHCH3CH2O)y(CH2CH2O)zR2NR3R4React at 60～70 DEG C with hydrogen peroxide,
Long-chain polyether nitrogen-containing compound is obtained Jing after processing；
(2) preparation of foam discharging agent compositionss
High salinity must be resisted to arrange the desired amount of long-chain polyether nitrogen-containing compound, fatty acid sulfoalkyl ester mix homogeneously
Hydromining gas foam discharging agent compositionss.
8. claim 1～6 arbitrary described anti-high salinity water pumping gas production application of foam discharging agent compositionss.
9. the anti-high salinity water pumping gas production according to claim 8 application of foam discharging agent compositionss, its
It is characterised by that the formation water salinity for being suitable for gas well is 0～250000mg/L.
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| CN109679605A (en) * | 2017-10-18 | 2019-04-26 | 中国石油化工股份有限公司 | Solid foam water discharge agent composition and preparation method and application |
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