CN103666411B - Fatty alcohol polyoxyethylene poly-oxygen propylene aether sulfonate compounds oil base emulsifying agent and preparation method thereof - Google Patents
Fatty alcohol polyoxyethylene poly-oxygen propylene aether sulfonate compounds oil base emulsifying agent and preparation method thereof Download PDFInfo
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Abstract
The present invention relates to a kind of fatty alcohol polyoxyethylene poly-oxygen propylene aether sulfonate and compound oil base emulsifying agent and preparation method thereof, mainly solve oil base drilling fluid emulsion-stabilizing performance problem poor, not salt tolerant, non-heatproof in prior art.The present invention is by the technical scheme of the compounding oil base emulsifying agent of fatty alcohol polyoxyethylene poly-oxygen propylene aether sulfonate, nonionic surfactant, anion surfactant, oil and water and preparation method thereof, preferably solve this problem, can be used for strong retraction, high-temperature stratum and need to bore in the Special Drilling Operation operations such as big displacement exceptional well, seaborne horizontal well.
Description
Technical field
The present invention relates to a kind of fatty alcohol polyoxyethylene poly-oxygen propylene aether sulfonate and compound oil base emulsifying agent and preparation thereof
Method.
Background technology
Along with constantly reducing and exploitation difficulty of petroleum reserves, countries in the world increase one after another to deep formation petroleum resources
The input of exploration and development, develops new oil reservoir and has become as an urgent demand of current each major oil companies development.China waits to verify
Petroleum resources be mainly distributed on Tarim Basin, Zhunger Basin, Qaidam, tell the basins such as Kazakhstan, Sichuan, the 73% of its stock number is imbedded in
Deep layer, and underground condition complex, therefore deep-well and ultradeep well oil gas drilling and supporting development technique have become restriction oil
The key factor of gas development of resources.Along with the increase of depth of stratum, deep-well, ultradeep well formation temperature also can be more and more higher, ground
Can the hot environment of layer maintain stable performance to bring challenge greatly to drilling fluid.
Drilling fluid is as the important component part of drilling engineering, and its performance is directly connected to the drilling well matter of deep-well, ultradeep well
Amount, drilling cost and drilling period.Relative to water-base drilling fluid, oil base drilling fluid has stronger anti-collapse inhibition, lubricity
With good reservoir protection performance, especially can meet strong retraction and high temperature, superhigh temperature stratum, or need to bore big displacement exceptional well
And seaborne horizontal well etc. is special turns drilling well needs.Oil base drilling fluid, also known as Water-In-Oil drilling fluid, is by oil, water, emulsifying agent, fall
Fluid loss agents, equilibrium of activation agent, flow pattern regulator etc. form.Normally used Water-In-Oil drilling fluid water content is between 5～30%
(water content generally referred to as full oil base drilling fluid, the most referred to as Water-In-Oil drilling fluid within 5%), but high temperature resistance reaches more than 180 DEG C
Water-In-Oil drilling fluid in the content of water typically 5～10%, rarely exceed 15%.The content of water increases, and takes bits property, filtration reduction
All improve with suspension, rheological characteristic, but heat stability and electrical stability are all deteriorated, as CN1660958 reports a kind of synthesis base
Drilling fluid, the primary emulsion of use is the mixture of AESA and NPE, although
Still having good rheological characteristic and emulsion-breaking voltage at 150 DEG C after aging 16 hours, water content is up to 25%, but higher temperature and water
Performance under content has no report.Oil base drilling fluid is owing to base fluid is based on oil, the most expensive, and cost is high, and full oil base bores
Well liquid is all the more so, and as CN101215461 reports a kind of complete-oil synthetic base drilling fluid, the emulsifying agent of use is Long carbon chain fat
The mixture of one or more in acid amide, Long carbon chain alkyl benzene calcium sulfonate, polyolefin carboxylic acid ester, although having low toxicity, ring
Protect, to advantages such as reservoir damage are little, but its preparation cost is high, limits it and promotes the use of.
There is provided in the market and be used as the of less types of oil base drilling fluid emulsifying agent, and report the breast for intensified oil reduction
Agent kind is the most, as US4485873, US4545912, CN100531884 etc. report polyoxyethylated alkyl phenol second
Hydrochlorate, double tail chain polyoxyethylene sulfonic acid salt, alkyl-fragrant benzyl-polyethenoxy ether anion surfactant answering in terms of intensified oil reduction
With, but it is not directed to its purposes in terms of well-drilling liquid emulgent.
Oil base drilling fluid is developed relatively slower owing to limiting by cost, environmental requirement always, and the block of application is the most relatively
Few, along with existing oilfield reserve declines day by day, and the exploitation in new exploratory area can run into various bad ground and environment, is badly in need of performance
Excellent prepares oil base drilling fluid emulsifying agent, and to solve, existing oil base drilling fluid emulsion-stabilizing performance is poor, not salt tolerant, non-heatproof
Problem.The Cost Problems of oil base drilling fluid is reduced, for extensively applying oil by improving the ratio of water in oil base drilling fluid
Base drilling fluid operation provides technical guarantee.In the case of the most this high-moisture described in invention, it is suitable for preparing stability and high efficiency
The preparation method of the oil base composite emulsifier of oil base drilling fluid.
Summary of the invention
One of the technical problem to be solved is that in prior art, oil base drilling fluid emulsion-stabilizing performance is poor, is weak to
Salt, the problem of non-heatproof, it is provided that a kind of new fatty alcohol polyoxyethylene poly-oxygen propylene aether sulfonate compounds oil base emulsifying agent.With
This fatty alcohol polyoxyethylene poly-oxygen propylene aether sulfonate compounds the oil base drilling fluid of oil base emulsifying agent preparation and has heat-resistant salt-resistant
The advantage that performance is good, emulsion-stabilizing performance is good.The two of the technical problem to be solved are to provide a kind of and solution technology
The corresponding fatty alcohol polyoxyethylene poly-oxygen propylene aether sulfonate of one of problem compounds the preparation method of oil base emulsifying agent.
In order to solve one of above-mentioned technical problem, the technical solution used in the present invention is as follows: a kind of fatty alcohol polyoxy second
Alkene polyoxypropylene ether sulfonate compounds oil base emulsifying agent, includes following component in terms of mass fraction:
The Fatty alcohol polyoxyethylene polyoxypropylene ether sulfonate of (1) 0.5～6 part；
The nonionic surfactant of (2) 0.5～5 parts；
The anion surfactant of (3) 0.1～3 parts；
The oil of (4) 5～50 parts；
The water of (5) 0.1～1 parts；
Wherein the general molecular formula of (1) component is:
In formula: M is any one ion in hydrogen, calcium, magnesium, barium, zinc, aluminum or ferrum, R is C8～C30Alkyl, m
For the adduction number of ethoxy group EO, its span is any one integer in 1～10, and n is the adduction number of propoxyl group group PO,
Its span is any one integer in 1～40, and x span is any one integer in 1～3.
In technique scheme, described ion preferred version is hydrogen, calcium, magnesium or zinc；R preferred version is C8～C20Alkane
Base；M preferred version is any one integer in 1～6；N preferred version is any one integer in 3～35；X preferred version
It is 1 or 2.Described nonionic surfactant preferred version is selected from this dish or tween or higher fatty acid amide.This described dish
At least one in this dish 20, this dish 40, this dish 60, span 80 or this dish 85 of series of surfactants preferred version；Tell
At least one in polysorbas20, polysorbate40, polysorbate60, Tween 80 or polysorbate85 of temperature series of surfactants preferred version；
Higher fatty acid amide series of surfactants preferred version is selected from lauroyl diethanolamine, cocos nucifera oil acyl diethanolamine, myristoyl
At least one in diethanolamine, palmitoleoyl diethanolamine, oleoyl diethanolamine or hard acyl diethanolamine.Described anion
Surfactant preferred version is sulfonates salt or long-chain alkyl benzene sulfonate.Described sulfonates salt
Preferred version is selected from carbon chain length C12～C18Sodium sulfate；Long-chain alkyl benzene sulfonate is selected from carbon chain length C12～C24Benzene sulfonic acid sodium salt；
Described oily preferred version is selected from white oil or liquid paraffin；Described water preferred version is selected from deionized water.
For solving the two of above-mentioned technical problem, the technical solution used in the present invention is as follows: a kind of fatty alcohol polyoxyethylene
Polyoxypropylene ether sulfonate compounds the preparation method of oil base emulsifying agent, comprises the following steps:
The preparation of (a) Fatty alcohol polyoxyethylene polyoxypropylene ether:
Being 85～160 DEG C by required proportioning in reaction temperature by fatty alcohol and oxirane, expoxy propane, pressure is less than
Under the conditions of 0.80MPa gauge pressure, calcium barium bimetallic compound is catalyst, reacts to obtain Fatty alcohol polyoxyethylene polyoxypropylene ether；Its
Middle fatty alcohol and oxirane, the mol ratio of expoxy propane are 1: 1～15: 1～50, and catalyst amount is fatty alcohol quality
1.0～8.0 %；
The preparation of (b) chloro fat alcohol polyoxyethylene poly-oxygen propylene aether:
Fatty alcohol polyoxyethylene polyoxypropylene ether synthesized by step (a) is pressed with thionyl chloride, pyridine by required proportioning
Required proportioning is reacted 3～10 hours at 70～100 DEG C, and the thionyl chloride of excess is extracted in decompression out, neutralizes layering and goes inorganic salt, vacuum
It is dried to obtain chloro fat alcohol polyoxyethylene poly-oxygen propylene aether；Wherein, Fatty alcohol polyoxyethylene polyoxypropylene ether, thionyl chloride and pyrrole
The mol ratio of pyridine is 1: 1～3: 0.5～2.5；
The preparation of (c) Fatty alcohol polyoxyethylene polyoxypropylene ether sulfonic acid (x=1)
Chloro fat alcohol polyoxyethylene poly-oxygen propylene aether synthesized by step (b) is placed in reactor, joins needed for addition
The mixture of the solvent 1,3-PD of ratio, sulfonating agent sodium sulfite or sodium sulfite and sodium sulfite and water, 90～150
At DEG C react 3～9 hours, then through steam water, neutralize, desalt to obtain Fatty alcohol polyoxyethylene polyoxypropylene ether sulfonic acid (x=1).Wherein,
Sulfonated reagent is the mixture of sodium sulfite or sodium sulfite and sodium sulfite, chloro fat alcohol polyoxyethylene poly-oxygen propylene aether
Being 1: 1.5～2.5 with the mol ratio of sulfonated reagent, 1,3-PD consumption is the 4～10% of reactant quality, and water consumption is anti-
Answer the 5～20% of material amount；
The preparation of (d) Fatty alcohol polyoxyethylene polyoxypropylene ether sulfonate (x=2 or 3)
By the Fatty alcohol polyoxyethylene polyoxypropylene ether sulfonic acid synthesized by step (c) by required proportioning and water, M (OH)xOr
MO(M2O3) be separately added in autoclave, it is 50～120 DEG C in reaction temperature, the response time is 0.5～5 hour, in 0.60MPa
Under the conditions of gauge pressure, react to obtain Fatty alcohol polyoxyethylene polyoxypropylene ether sulfonate；Wherein Fatty alcohol polyoxyethylene polyoxypropylene ether
The mol ratio of sulfonic acid and hydroxide or oxide is 1.5～3: 1, and water accounts for that to react the mass percent of total material be 60～90%,
M(OH)xOr MO (M2O3) Average Particle Diameters be 200nm～200 μm；
E () is by the desired amount of Fatty alcohol polyoxyethylene polyoxypropylene ether sulfonate, nonionic surfactant, anion table
Face activating agent, base oil and water are sequentially added in reaction bulb, are warming up to 30～80 DEG C and stir 1～4 hour, obtain required compounding
Oil base emulsifying agent.In terms of mass fraction, Fatty alcohol polyoxyethylene polyoxypropylene ether sulfonate, nonionic surfactant, cloudy from
The proportioning of sub-surface activating agent, oil and water is 0.5～6 part: 0.5～5 part: 0.1～3 part: 5～50 parts: 0.5～3 part.
In technique scheme, the preferred scope of reaction temperature in (a) step is 120～160 DEG C, the preferred scope of pressure
It it is 0.30～0.60MPa gauge pressure；Fatty alcohol and oxirane, expoxy propane mole preferably ratio for 1: 1～5: 5～35, catalysis
Agent consumption is preferably the 2.5～5.0% of fatty alcohol quality；Fatty alcohol polyoxyethylene polyoxypropylene ether, thionyl chloride in (b) step
Being preferably 1: 1.5～2.5: 1～2 with the mol ratio of pyridine, reaction temperature is preferably 75～90 DEG C, and the response time is preferably 4～8
Hour；C in () step, chloro fat alcohol polyoxyethylene poly-oxygen propylene aether is preferably 1: 1.5～2 with the mol ratio of sulfonated reagent,
1,3-PD consumption is preferably the 5～8% of reactant quality, and water consumption is preferably the 10～15% of reactant quality, reaction temperature
Degree is preferably 110～140 DEG C, and the response time is preferably 4～8 hours；Fatty alcohol polyoxyethylene polyoxypropylene ether in (d) step
Sulfonic acid and M (OH)xOr MO (M2O3) mol ratio be preferably 1.8～2.5: 1, water accounts for that to react the mass percent of total material preferred
It is 70～85%, M (OH)xOr MO (M2O3) Average Particle Diameters be preferably 400nm～100 μm, reaction temperature be preferably 60～
90 DEG C, the response time is preferably 1～3 hour；(e) in terms of mass fraction, Fatty alcohol polyoxyethylene polyoxypropylene ether sulfonate
The preferred scope of consumption is 1～4 part, and the preferred scope of consumption of nonionic surfactant is 1～4 part, anion surfactant
The preferred scope of consumption be 0.5～1 part, oil the preferred scope of consumption be 10～40 parts, the preferred scope of consumption of water be 0.3～
0.7 part, reaction temperature is preferably 40～70 DEG C, and mixing time is preferably 2～3 hours.
Fatty alcohol polyoxyethylene poly-oxygen propylene aether sulfonate prepared by the present invention compounds oil base emulsifying agent, due to fatty alcohol
Polyoxyethylene poly-oxygen propylene aether sulfonate molecules structure contains polyoxyethylene, polyoxypropylene non-ionic group and sulfonate radical simultaneously
Anionic group so that it is have the heat resistance of anion surfactant and the salt tolerant advantage of nonionic surfactant concurrently, with
Time each surfactant between there is well collaborative Emulsification effect, be a kind of oil base drilling fluid being suitable for high temperature and high salt stratum
With compounding oil base emulsifying agent.
The fatty alcohol polyoxyethylene poly-oxygen propylene aether sulfonate using the present invention to prepare compounds the oil base of oil base emulsifying agent
Drilling fluid, it mainly comprises and includes following component: base oil 70～90 parts, water 10～30 parts, emulsifying agent 1～5 parts, organoclay 2
～5 parts, fluid loss additive 0.5～3 parts, pH adjusting agent 0.5～3 parts.This oil base drilling fluid heatproof reach 180 DEG C, API filtration≤
Emulsion-breaking voltage >=800V before and after 3ml, high temperature ageing, is that a kind of heat-resistant salt-resistant function admirable, filter loss be little, good emulsion stability
Oil base drilling fluid system, achieves preferable technique effect.
Accompanying drawing explanation
Fig. 1 is the infrared spectrogram of Fatty alcohol polyoxyethylene polyoxypropylene ether sulfonic acid (x=1).
Fig. 2 is the infrared spectrogram of Fatty alcohol polyoxyethylene polyoxypropylene ether sulfonate (x=2 or 3).
Fatty alcohol polyoxyethylene polyoxypropylene ether sulfonic acid and salt prepared by the present invention can characterize by the following method: will synthesis
After thing purifies, application U.S. Nicolet-380 FT-IR spectrogrph, use pressing potassium bromide troche or liquid-film method to carry out infrared spectrum
Analyze (sweep limits 4000～400cm-1), determine the chemical constitution of sample, to reach compound of the present invention
Infrared Characterization.
As shown in Figure 1, wave number 2921cm-1、2851cm-1For methyl on alkyl chain and methylene C-H telescope features peak,
Wave number 725 cm-1The characteristic peak waved in chain alkyl C-H face occurs；Wave number 1713cm-1Characteristic absorption peak for carboxylic acid；
1350cm-1The characteristic peak that peak is sulfonate of left and right, is owing to antisymmetric stretching vibration and the vibration of skeleton carbon of S=O cause；
Wave number 1115cm-1Absworption peak for C-O-C key.
As shown in Figure 2, wave number 2915cm-1、2860cm-1For methyl on alkyl chain and methylene C-H telescope features peak,
Wave number 725 cm-1The characteristic peak waved in chain alkyl C-H face occurs；Wave number 1616cm-1Characteristic absorption peak for carboxylate；
1352cm-1Peak, left and right is the characteristic peak of sulfonate, is owing to antisymmetric stretching vibration and the vibration of skeleton carbon of S=O cause；Ripple
Number 1110cm-1Absworption peak for C-O-C key.
Below by embodiment, the present invention is further elaborated.
Detailed description of the invention
[embodiment 1]
The synthesis of (a) lauryl alcohol polyoxyethylene poly-oxygen propylene aether (m=3, n=15)
Add in the reactor equipped with condensing unit, agitating device and gas distributor 186 grams of (1 mole) lauryl alcohols,
3.0 grams of calcium oxide and 2.6 grams of Barium monoxides, while lead to nitrogen limit when being heated to 135 DEG C, add 20 grams of water, stirring reaction 1 hour.De-
After moisture removal, being cooled to 80 DEG C, slowly the sulphuric acid (20wt%) of dropping catalyst neutralisation theoretical amount prepares high activity, high selectivity
Calcium barium bimetallic catalyst reactant liquor system, system temperature is heated to 80～90 DEG C, open vacuum system, under a high vacuum
It is dehydrated 2 hours, then purges 3～4 times with nitrogen, system reaction temperature is adjusted to 150 DEG C and is slowly passed through 132 grams of (3 moles) rings
Oxidative ethane, controls pressure≤0.40MPa, after reacting ethylene oxide terminates, is that 150 DEG C are slowly passed through 870 grams (15 moles)
Expoxy propane, controls pressure≤0.50MPa.After reaction terminates, purge system with nitrogen, neutralize after cooling, be dehydrated, obtain lauryl alcohol
Polyoxyethylene poly-oxygen propylene aether (m=3, n=15) 1141.7 grams, molar yield 96.1%.
The synthesis of (b) chloro lauryl alcohol polyoxyethylene poly-oxygen propylene aether (m=3, n=15)
By the lauryl alcohol polyoxyethylene poly-oxygen propylene aether (m=3, n=15) 1141.7 grams synthesized by step (a), (0.961 rubs
You), 75.9 grams of (0.961 mole) pyridines be placed in equipped with backflow, stirring, gas absorbing device 2000 milliliters of there-necked flasks in,
The most slowly dropping thionyl chloride 171.5 grams (1.442 moles), reacts 6 hours at 80 DEG C, and reaction is reduced pressure after terminating and boiled off
Excess thionyl chloride, residue cooling, stratification, upper strata is neutralized to neutrality with the sodium hydroxide solution of 30%, divide go inorganic
Salt, organic layer is washed with water to be washed 3～4 times, is vacuum dried to obtain chloro lauryl alcohol polyoxyethylene poly-oxygen propylene aether (m=3, n=15)
1035.4 gram, molar yield 89.3%.
The synthesis of (c) lauryl alcohol polyoxyethylene poly-oxygen propylene aether isopropyl sulfonic acid (m=3, n=15)
By chloro lauryl alcohol polyoxyethylene poly-oxygen propylene aether (m=3, n=15) synthesized by step (b) 1035.4 gram (0.858
Mole) be placed in autoclave, add 62.1 grams of 1,3-PDs, 124.3 grams of water, (1.240 rub 156.3 grams of sodium sulfite
You) and 31.7 grams of sodium sulfitees (0.305 mole), to react 6 hours at a temperature of 120 DEG C, after reaction terminates, decompression distillation is steamed
To go most of moisture, mixture adds appropriate isopropanol and stands overnight, filter the inorganic salt being precipitated out. decompression is removed molten
Agent, cooling, neutralize, add q. s. methylene chloride and further filter out inorganic salt, obtain lauryl alcohol polyoxyethylene poly-oxygen propylene aether different
Propane sulfonic acid (m=3, n=15) 914.2 grams, molar yield is 85.1%.
The synthesis of (d) lauryl alcohol polyoxyethylene poly-oxygen propylene aether isopropyl sulfoacid calcium (m=3, n=15)
To being furnished with in churned mechanically high-pressure reactor the lauryl alcohol polyoxyethylene polyoxy being separately added into synthesized by step (c)
Propylene ether isopropyl sulfonic acid (m=3, n=15) 914.2 grams (0.730 mole), 20.4 grams of (0.365 mole) CaO (Average Particle Diameters
It is 40 μm) and 3738.4 grams of water, it is heated to 70 DEG C, logical nitrogen makes system pressure be that to react 2.5 under the conditions of 0.60MPa gauge pressure little
Time, after reaction terminates, cooling, branch vibration layer, product is dried, is obtained lauryl alcohol polyoxyethylene poly-oxygen propylene aether isopropyl sulfoacid calcium (m=
3, n=15) 909.4 grams.
Lauryl alcohol polyoxyethylene poly-oxygen propylene aether isopropyl sulfoacid calcium (m=3, n=15) to synthesis, applies U.S. Nicolet-
5700 infrared spectrometers, use pressed disc method to carry out infrared spectrum analysis (sweep limits 4000～400cm-1), have shown in Fig. 2
Characteristic peak.
E () by percentage to the quality, takes lauryl alcohol polyoxyethylene poly-oxygen propylene aether isopropyl sulfoacid calcium (m=3, the n=of synthesis
15) 3 parts, 85 1 parts of this dish, sodium lauryl sulphate 0.5 part, 0.5 part and 30 parts liquid paraffin of water be sequentially added in reaction bulb,
Being warming up to 60 DEG C stir 3 hours, obtain required compounding oil base emulsifying agent oil solution, wherein compound emulsion agent content is with quality hundred
Proportion by subtraction is calculated as 12.9%.
[embodiment 2]
The synthesis of (a) hexadecanol polyoxyethylene poly-oxygen propylene aether (m=2, n=6)
Add in the reactor equipped with condensing unit, agitating device and gas distributor 242 grams of (1 mole) hexadecanol,
4.5 grams of calcium oxide and 3.0 grams of Barium monoxides, while lead to nitrogen limit when being heated to 135 DEG C, add 20 grams of water, stirring reaction 1 hour.De-
After moisture content, being cooled to 80 DEG C, slowly the sulphuric acid (20wt%) of dropping catalyst neutralisation theoretical amount prepares high activity, high selectivity
Compositional type calcium barium bimetallic catalyst reactant liquor system, system temperature is heated to 80～90 DEG C, open vacuum system, at height
Dehydrated under vacuum 2 hours, then purges 3～4 times with nitrogen, system reaction temperature is adjusted to 140 DEG C and is slowly passed through 88 grams (2 rub
You) oxirane, control pressure≤0.40MPa, after reacting ethylene oxide terminates, be that 160 DEG C are slowly passed through 348 grams (6 rub
You) expoxy propane, control pressure≤0.60MPa.After reaction terminates, purge system with nitrogen, neutralize after cooling, be dehydrated, obtain ten
Six alcohol polyoxyethylene poly-oxygen propylene aethers (m=2, n=6) 659.0 grams, molar yield 97.2 %.
The synthesis of (b) chloro hexadecanol polyoxyethylene poly-oxygen propylene aether (m=2, n=6)
By the hexadecanol polyoxyethylene poly-oxygen propylene aether (m=2, n=6) 659.0 grams synthesized by step (a), (0.972 rubs
You), 115.2 grams of (1.458 moles) pyridines are placed in equipped with backflow, stirring, 2000 milliliters of there-necked flasks of gas absorbing device
In, the most slowly dropping thionyl chloride 231.3 grams (1.944 moles), to react 8 hours at 75 DEG C, reaction terminates post processing
With [embodiment 1] (b), obtain chloro hexadecanol polyoxyethylene poly-oxygen propylene aether (m=2, n=6) 586.3 grams, molar yield 86.6%.
The synthesis of (c) hexadecanol polyoxyethylene poly-oxygen propylene aether isopropyl sulfonic acid (m=2, n=6)
By chloro hexadecanol polyoxyethylene poly-oxygen propylene aether (m=2, n=6) 586.3 grams synthesized by step (b), (0.842 rubs
You) it is placed in autoclave, add 46.9 grams of 1,3-PDs, 87.9 grams of water, 170.1 grams of sodium sulfite (1.350 moles)
And 34.5 grams of sodium sulfitees (0.332 mole), to react 7 hours at a temperature of 130 DEG C, remaining operation is same [embodiment 1] (c),
Obtaining hexadecanol polyoxyethylene poly-oxygen propylene aether isopropyl sulfonic acid (m=2, n=6) 529.8 grams, molar yield is 84.8%.
The synthesis of (d) hexadecanol polyoxyethylene poly-oxygen propylene aether isopropyl sulfonic acid zinc (m=2, n=6)
To being furnished with in churned mechanically high-pressure reactor the hexadecanol polyoxyethylene polyoxy being separately added into synthesized by step (c)
Propylene ether isopropyl sulfonic acid (m=2, n=6) 529.8 grams (0.714 mole), (Average Particle Diameters is 32.3 grams of (0.397 mole) CaO
500nm) He 3185.2 grams of water, are heated to 65 DEG C, and logical nitrogen makes system pressure be to react 3 hours under the conditions of 0.60MPa gauge pressure, instead
After should terminating, cooling, branch vibration layer, product is dried, is obtained hexadecanol polyoxyethylene poly-oxygen propylene aether isopropyl sulfonic acid zinc (m=2, n=6)
542.6 gram.
Hexadecanol polyoxyethylene poly-oxygen propylene aether isopropyl sulfonic acid zinc (m=2, n=6) to synthesis, applies U.S. Nicolet-
5700 infrared spectrometers, use pressed disc method to carry out infrared spectrum analysis (sweep limits 4000～400cm-1), have shown in Fig. 2
Characteristic peak.
E () by percentage to the quality, takes hexadecanol polyoxyethylene poly-oxygen propylene aether isopropyl sulfonic acid zinc (m=2, the n=of synthesis
6) 3 parts, polysorbate40 0.5 part, 0.5 part of cetyl benzenesulfonic acid sodium, 0.3 part and 30 parts liquid paraffin of water be sequentially added into reaction bulb
In, it is warming up to 70 DEG C and stirs 2 hours, obtain required compounding oil base emulsifying agent oil solution, wherein compound emulsion agent content is with matter
Amount percentages is 11.7%.
[embodiment 3]
The synthesis of (a) capryl alcohol polyoxyethylene poly-oxygen propylene aether (m=1, n=35)
Add in the reactor equipped with condensing unit, agitating device and gas distributor 130 grams of (1 mole) capryl alcohol, 3.7
Gram calcium oxide and 3.0 grams of Barium monoxides, while lead to nitrogen limit when being heated to 135 DEG C, add 25 grams of water, stirring reaction 1 hour.Removing water
After Fen, being cooled to 80 DEG C, slowly the sulphuric acid (20wt%) of dropping catalyst neutralisation theoretical amount prepares high activity, high selective calcium
Barium bimetallic catalyst reactant liquor system, is heated to 80～90 DEG C by system temperature, opens vacuum system, is dehydrated under a high vacuum
2 hours, then purge 3～4 times with nitrogen, system reaction temperature is adjusted to 120 DEG C and is slowly passed through 44 grams of (1 mole) epoxy second
Alkane, controls pressure≤0.40MPa, after reacting ethylene oxide terminates, is that 150 DEG C are slowly passed through 2030 grams of (35 moles) epoxies
Propane, controls pressure≤0.50MPa.After reaction terminates, purge system with nitrogen, neutralize after cooling, be dehydrated, obtain capryl alcohol polyoxy second
Alkene polyethenoxy ether (m=1, n=35) 2126.9 grams, molar yield 96.5%.
The synthesis of (b) chloro capryl alcohol polyoxyethylene poly-oxygen propylene aether (m=1, n=35)
By the capryl alcohol polyoxyethylene poly-oxygen propylene aether (m=1, n=35) 1102.0 grams (0.5 mole) synthesized by step (a),
71.1 grams of (0.9 mole) pyridines be placed in equipped with backflow, stirring, gas absorbing device 2000 milliliters of there-necked flasks in, in stirring
Under slowly drip thionyl chloride 119.0 grams (1.0 moles), react 4 hours at 85 DEG C, reaction terminates post processing with [embodiment 1]
B (), obtains chloro capryl alcohol polyoxyethylene poly-oxygen propylene aether (m=1, n=35) 891.2 grams, molar yield 80.2%.
The synthesis of (c) capryl alcohol polyoxyethylene poly-oxygen propylene aether isopropyl sulfonic acid (m=1, n=35)
By chloro capryl alcohol polyoxyethylene poly-oxygen propylene aether (m=1, n=35) 891.2 grams (0.4 mole) synthesized by step (b)
Be placed in autoclave, add 44.6 grams of 1,3-PDs, 89.1 grams of water, 60.6 grams of sodium sulfite (0.481 mole) and
12.3 grams of sodium sulfitees (0.118 mole), react 4 hours at a temperature of 140 DEG C, and remaining operation, with [embodiment 1] (c), obtains
Capryl alcohol polyoxyethylene poly-oxygen propylene aether isopropyl sulfonic acid (m=1, n=35) 730.3 grams, molar yield is 80.5%.
Capryl alcohol polyoxyethylene poly-oxygen propylene aether isopropyl sulfonic acid (m=1, n=35) to synthesis, applies U.S. Nicolet-5700
Infrared spectrometer, uses liquid-film method to carry out infrared spectrum analysis (sweep limits 4000～400cm-1), there is the feature shown in Fig. 1
Peak.
E () by percentage to the quality, takes capryl alcohol polyoxyethylene poly-oxygen propylene aether isopropyl sulfonic acid (m=1, n=35) 1 of synthesis
Part, 40 4 parts of this dish, sodium lauryl sulphate 0.5 part, 0.5 part and 10 parts liquid paraffin of water are sequentially added in reaction bulb, heat up
Stirring 2 hours to 50 DEG C, obtain required compounding oil base emulsifying agent oil solution, wherein compound emulsion agent content is with mass percent
It is calculated as 34.4%.
[embodiment 4]
The synthesis of (a) octodecyl alcohol polyoxyethylene polyethenoxy ether (m=5, n=8)
Add in the reactor equipped with condensing unit, agitating device and gas distributor 270 grams of (1 mole) octadecanol,
5.0 grams of calcium oxide and 3.1 grams of Barium monoxides, while lead to nitrogen limit when being heated to 135 DEG C, add 25 grams of water, stirring reaction 1 hour.De-
After moisture content, being cooled to 80 DEG C, slowly the sulphuric acid (20wt%) of dropping catalyst neutralisation theoretical amount prepares high activity, high selectivity
Calcium barium bimetallic catalyst reactant liquor system, system temperature is heated to 80～90 DEG C, open vacuum system, under a high vacuum
It is dehydrated 2 hours, then purges 3～4 times with nitrogen, system reaction temperature is adjusted to 130 DEG C and is slowly passed through 220 grams of (5 moles) rings
Oxidative ethane, controls pressure≤0.40MPa, after reacting ethylene oxide terminates, is that 150 DEG C are slowly passed through 464 grams of (8 moles) rings
Ethylene Oxide, controls pressure≤0.50MPa.After reaction terminates, purge system with nitrogen, neutralize after cooling, be dehydrated, obtain octadecanol and gather
Oxygen ethylene polyethenoxy ether (m=5, n=8) 937.8 grams, molar yield 98.3%.
The synthesis of (b) chloro octodecyl alcohol polyoxyethylene polyethenoxy ether (m=5, n=8)
By the octodecyl alcohol polyoxyethylene polyethenoxy ether (m=5, n=8) 937.8 grams (0.983 mole) synthesized by step (a)
, 93.2 grams of (1.180 moles) pyridines be placed in equipped with backflow, stirring, gas absorbing device 2000 milliliters of there-necked flasks in, stirring
Mixing down and slowly drip thionyl chloride 175.5 grams (1.475 moles), react 5 hours at 90 DEG C, reaction terminates post processing with [implementing
Example 1] (b), obtain chloro octodecyl alcohol polyoxyethylene polyethenoxy ether (m=5, n=8) 865.2 grams, molar yield 90.5%.
The synthesis of (c) octodecyl alcohol polyoxyethylene polyethenoxy ether isopropyl sulfonic acid (m=5, n=8)
By chloro octodecyl alcohol polyoxyethylene polyethenoxy ether (m=5, n=8) 865.2 grams synthesized by step (b), (0.890 rubs
You) it is placed in autoclave, add 69.2 grams of 1,3-PDs, 121.1 grams of water, 143.9 grams of sodium sulfite (1.143 moles)
And 29.2 grams of sodium sulfitees (0.281 mole), to react 8 hours at a temperature of 110 DEG C, remaining operation is same [embodiment 1] (c),
Obtaining octodecyl alcohol polyoxyethylene polyethenoxy ether isopropyl sulfonic acid (m=5, n=8) 760.2 grams, molar yield is 83.9%.
The synthesis of (d) octodecyl alcohol polyoxyethylene polyethenoxy ether isopropyl sulfoacid calcium (m=5, n=8)
To being furnished with in churned mechanically high-pressure reactor the octodecyl alcohol polyoxyethylene polyoxy being separately added into synthesized by step (c)
Propylene ether isopropyl sulfonic acid (m=5, n=8) 760.2 grams (0.747 mole), 24.1 grams of (0.325 mole) Ca (OH)2(mean diameter is big
Little is 80 μm) and 1830.0 grams of water, it is heated to 85 DEG C, logical nitrogen makes system pressure be that to react 1.5 under the conditions of 0.60MPa gauge pressure little
Time, after reaction terminates, cooling, branch vibration layer, product is dried, is obtained octodecyl alcohol polyoxyethylene polyethenoxy ether isopropyl sulfoacid calcium (m=
5, n=8) 762.9 grams.
Octodecyl alcohol polyoxyethylene polyethenoxy ether isopropyl sulfoacid calcium (m=5, n=8) to synthesis, applies U.S. Nicolet-
5700 infrared spectrometers, use pressed disc method to carry out infrared spectrum analysis (sweep limits 4000～400cm-1), have shown in Fig. 2
Characteristic peak.
E () by percentage to the quality, takes octodecyl alcohol polyoxyethylene polyethenoxy ether isopropyl sulfoacid calcium (m=5, the n=of synthesis
8) 1 part, 60 3 parts of this dish, sodium lauryl sulphate 1 part, 0.8 part and 40 parts liquid paraffin of water be sequentially added in reaction bulb, heat up
Stirring 3 hours to 60 DEG C, obtain required compounding oil base emulsifying agent oil solution, wherein compound emulsion agent content is with mass percent
It is calculated as 10.9%.
[embodiment 5]
The synthesis of (a) lauryl alcohol polyoxyethylene poly-oxygen propylene aether (m=3, n=30)
Add in the reactor equipped with condensing unit, agitating device and gas distributor 186 grams of (1 mole) lauryl alcohols,
5.7 grams of calcium oxide and 3.6 grams of Barium monoxides, while lead to nitrogen limit when being heated to 135 DEG C, add 30 grams of water, stirring reaction 1 hour.De-
After moisture content, being cooled to 80 DEG C, slowly the sulphuric acid (20wt%) of dropping catalyst neutralisation theoretical amount prepares high activity, high selectivity
Calcium barium bimetallic catalyst reactant liquor system, system temperature is heated to 80～90 DEG C, open vacuum system, under a high vacuum
It is dehydrated 2 hours, then purges 3～4 times with nitrogen, system reaction temperature is adjusted to 130 DEG C and is slowly passed through 132 grams of (3 moles) rings
Oxidative ethane, controls pressure≤0.40MPa, after reacting ethylene oxide terminates, is that 160 DEG C are slowly passed through 1740 grams (30 moles)
Expoxy propane, controls pressure≤0.60MPa.After reaction terminates, purge system with nitrogen, neutralize after cooling, be dehydrated, obtain lauryl alcohol
Polyoxyethylene poly-oxygen propylene aether (m=3, n=30) 1938.6 grams, molar yield 94.2%.
The synthesis of (b) chloro lauryl alcohol polyoxyethylene poly-oxygen propylene aether (m=3, n=30)
By the lauryl alcohol polyoxyethylene poly-oxygen propylene aether (m=3, n=30) 1029.0 grams (0.5 mole) synthesized by step (a)
, 79.0 grams of (1.0 moles) pyridines be placed in equipped with backflow, stirring, gas absorbing device 2000 milliliters of there-necked flasks in, in stirring
Under slowly drip thionyl chloride 148.8 grams (1.25 moles), react 7 hours at 75 DEG C, reaction terminates post processing with [embodiment 1]
B (), obtains chloro lauryl alcohol polyoxyethylene poly-oxygen propylene aether (m=3, n=30) 850.3 grams, molar yield 81.9%.
The synthesis of (c) lauryl alcohol polyoxyethylene poly-oxygen propylene aether isopropyl sulfonic acid (m=3, n=30)
By chloro lauryl alcohol polyoxyethylene poly-oxygen propylene aether (m=3, n=30) synthesized by step (b) 850.3 gram (0.409
Mole) be placed in autoclave, add 59.5 grams of 1,3-PDs, 127.5 grams of water, (0.591 rubs 74.4 grams of sodium sulfite
You) and 15.1 grams of sodium sulfitees (0.145 mole), to react 7 hours at a temperature of 120 DEG C, remaining operation is with [embodiment 1]
C (), obtains lauryl alcohol polyoxyethylene poly-oxygen propylene aether isopropyl sulfonic acid (m=3, n=30) 683.0 grams, molar yield is 78.7%.
Lauryl alcohol polyoxyethylene poly-oxygen propylene aether isopropyl sulfonic acid (m=3, n=30) to synthesis, applies U.S. Nicolet-
5700 infrared spectrometers, use liquid-film method to carry out infrared spectrum analysis (sweep limits 4000～400cm-1), have shown in Fig. 1
Characteristic peak.
D () by percentage to the quality, takes lauryl alcohol polyoxyethylene poly-oxygen propylene aether isopropyl sulfonic acid (m=3, n=30) of synthesis
4 parts, lauroyl diethanolamine 0.5 part, sodium hexadecyl sulfate 0.5 part, 0.3 part and 10 parts liquid paraffin of water be sequentially added into reaction
In Ping, be warming up to 40 DEG C and stir 2 hours, obtain required compounding oil base emulsifying agent oil solution, wherein compound emulsion agent content with
Mass percent is calculated as 32.7%.
[embodiment 6]
With [embodiment 1], difference substitutes 1 part of this dish 85 with 1 part of hard acyl diethanolamine, and remaining is identical, obtains required
Compounding oil base emulsifying agent oil solution.
[embodiment 7]
With [embodiment 1], the usage amount of lauryl alcohol polyoxyethylene poly-oxygen propylene aether isopropyl sulfoacid calcium (m=3, n=15) is 4
Part, difference substitutes 1 part of this dish 85 with 0.5 part of polysorbate85, and remaining is identical, obtains required compounding oil base emulsifying agent oil soluble
Liquid.
[embodiment 8～14]
The compounding oil base emulsifying agent preparation oil base drilling fluid system synthesized with [embodiment 1～7], the oil-water ratio of employing is
70:30, basic recipe is 210mL oil+90mL 20wt%CaCl2Aqueous solution+3wt % compound emulsifying agent+3 wt % organoclay+
1wt % organic amine modified humic acid+1 wt % butadiene rubber+1 wt % CaO powder.Wherein, white oil total amount comprises compound emulsion
White oil amount in agent oil solution, the addition of composite emulsifier is converted with the mass percent of composite emulsifier oil solution.
Accurately weigh a certain amount of white oil and 3 wt % emulsifying agents mixing (total amount of white oil is 210mL), high-speed stirred
10min, sequentially adds 3 wt % organoclays, 1wt % organic amine modified humic acid, 1 wt % EP rubbers and 1 wt % CaO
Powder, continues high-speed stirred 20min, is eventually adding 90mL 20wt%CaCl2Aqueous solution, then high-speed stirred 10min, stablized
Water-in-oil type drilling fluid system.Measure the rheological parameter of this water-in-oil type drilling fluid system, emulsion-breaking voltage and API leak-off respectively
Amount.Wherein rheological parameter uses Qingdao Cacumen et folium clerodendri mandarinori (Clerodendron mandarinorum Diels) to reach the ZNN-D6 type six speed rotary viscosity design determining of instrumentation factory, and according to public affairs
Formula (1) and (2) calculate apparent viscosity (μa) and plastic viscosity (μp), emulsion-breaking voltage is by the DWY-2 of Qingdao sensible instrumentation factory
Type drilling fluid electrical stability analyzer measures, and API filtration is measured by the multi-joint filtration device of SD type, and calculates according to formula (3)
Filter loss (FL).
Formula (1)(mPa.s)
Formula (2) (mPa.s)
Formula (3) (mL)
Being put in XGRL-4 type high temp roller heating furnace by the above-mentioned water-in-oil type drilling fluid prepared, 180 DEG C of high temperature are old
Change 24 hours, measure the rheological parameter of this water-in-oil type drilling fluid system, emulsion-breaking voltage and API filtration, instrument respectively
And process is with before aging, result is as shown in table 1,2.
Oil base drilling fluid system performance before table 1 aged at room temperature
2 180 DEG C of table is oil base drilling fluid system performance after aging 24 hours
[comparative example 1]
With [embodiment 8], difference uses 3 wt % calcium stearates to substitute the compounding oil of 3 wt % prepared by [embodiment 1]
Base emulsifying agent is emulsifying agent, and remaining is identical, determines the rheological parameter of water-in-oil type drilling fluid system, emulsion-breaking voltage and API filter
Vector, result is as shown in table 3.
Table 3
Claims (8)
1. fatty alcohol polyoxyethylene poly-oxygen propylene aether sulfonate compounds an oil base emulsifying agent, includes following in terms of mass fraction
Component:
The Fatty alcohol polyoxyethylene polyoxypropylene ether sulfonate of (1) 0.5～6 part；
The nonionic surfactant of (2) 0.5～5 parts；
The anion surfactant of (3) 0.1～3 parts；
The oil of (4) 5～50 parts；
The water of (5) 0.1～1 parts；
Wherein the general molecular formula of (1) component is:
In formula: M is any one ion in calcium, magnesium, barium, zinc, aluminum or ferrum, R is C8～C30Alkyl, m is ethyoxyl
The adduction number of group EO, its span is any one integer in 1～10, and n is the adduction number of propoxyl group group PO, its value model
Enclosing is any one integer in 1～40, and x span is any one integer in 2 or 3.
Fatty alcohol polyoxyethylene poly-oxygen propylene aether sulfonate the most according to claim 1 compounds oil base emulsifying agent, and it is special
Levy and be that described ion is calcium, magnesium or zinc；R is C8～C20Alkyl；M is any one integer in 1～6；N is in 3～35
Any one integer；X is 2.
Fatty alcohol polyoxyethylene poly-oxygen propylene aether sulfonate the most according to claim 1 compounds oil base emulsifying agent, and it is special
Levy and be that described nonionic surfactant is selected from this dish or tween or higher fatty acid amide；Wherein, higher fatty acid amide choosing
From lauroyl diethanolamine, cocos nucifera oil acyl diethanolamine, myristoyl diethanolamine, palmitoleoyl diethanolamine, oleoyl diethanol
At least one in amine or stearoyl diethanolamine.
Fatty alcohol polyoxyethylene poly-oxygen propylene aether sulfonate the most according to claim 3 compounds oil base emulsifying agent, and it is special
Levy and be that this described dish series of surfactants is selected from this dish 20, this dish 40, this dish 60, span 80 or this dish 85 at least
A kind of；At least one in polysorbas20, polysorbate40, polysorbate60, Tween 80 or polysorbate85 of TWEEN Series surfactant.
Fatty alcohol polyoxyethylene poly-oxygen propylene aether sulfonate the most according to claim 1 compounds oil base emulsifying agent, and it is special
Levy and be that described anion surfactant is sulfonates salt or long-chain alkyl benzene sulfonate；Wherein, described
Sulfonates salt is selected from carbon chain length C12～C18Sodium sulfate；Long-chain alkyl benzene sulfonate is selected from carbon chain length C12～C24's
Benzene sulfonic acid sodium salt.
Fatty alcohol polyoxyethylene poly-oxygen propylene aether sulfonate the most according to claim 5 compounds oil base emulsifying agent, and it is special
Levy and be that described grease separation is from white oil；Described wet concentration is from deionized water.
7. the fatty alcohol polyoxyethylene poly-oxygen propylene aether sulfonate described in claim 1 compounds the preparation side of oil base emulsifying agent
Method, comprises the following steps:
The preparation of (a) Fatty alcohol polyoxyethylene polyoxypropylene ether:
Being 85～160 DEG C by required proportioning in reaction temperature by fatty alcohol and oxirane, expoxy propane, pressure is less than
Under the conditions of 0.80MPa gauge pressure, calcium barium bimetallic compound is catalyst, reacts to obtain Fatty alcohol polyoxyethylene polyoxypropylene ether；Its
Middle fatty alcohol and oxirane, the mol ratio of expoxy propane are 1: 1～15: 1～50, and catalyst amount is fatty alcohol quality
1.0～8.0%；
The preparation of (b) chloro fat alcohol polyoxyethylene poly-oxygen propylene aether:
Fatty alcohol polyoxyethylene polyoxypropylene ether synthesized by step (a) is pressed required by required proportioning with thionyl chloride, pyridine
Proportioning is reacted 3～10 hours at 70～100 DEG C, and the thionyl chloride of excess is extracted in decompression out, neutralizes layering and removes inorganic salt, vacuum drying
Obtain chloro fat alcohol polyoxyethylene poly-oxygen propylene aether；Wherein, Fatty alcohol polyoxyethylene polyoxypropylene ether, thionyl chloride and pyridine
Mol ratio is 1: 1～3: 0.5～2.5；
The preparation of (c) Fatty alcohol polyoxyethylene polyoxypropylene ether sulfonic acid
Chloro fat alcohol polyoxyethylene poly-oxygen propylene aether synthesized by step (b) is placed in reactor, adds required proportioning
Solvent 1,3-PD, sulfonated reagent and water, at 90～150 DEG C react 3～9 hours, then through steam water, neutralize, desalt to obtain fat
Fat alcohol polyoxyethylene poly-oxygen propylene aether sulfonic acid；Wherein, what sulfonated reagent was sodium sulfite or sodium sulfite with sodium sulfite is mixed
Compound, chloro fat alcohol polyoxyethylene poly-oxygen propylene aether is 1: 1.5～2.5 with the mol ratio of sulfonated reagent, and 1,3-PD is used
Amount is the 4～10% of reactant quality, and water consumption is the 5～20% of reactant quality；
The preparation of (d) Fatty alcohol polyoxyethylene polyoxypropylene ether sulfonate
By the Fatty alcohol polyoxyethylene polyoxypropylene ether sulfonic acid synthesized by step (c) by required proportioning and water, the oxide of M or hydrogen
Oxide is separately added in autoclave, is 50～120 DEG C in reaction temperature, and the response time is 0.5～5 hour, in 0.60MPa table
Under the conditions of pressure, react to obtain Fatty alcohol polyoxyethylene polyoxypropylene ether sulfonate；Wherein Fatty alcohol polyoxyethylene polyoxypropylene ether sulphur
Acid is 1.5～3: 1 with the mol ratio of hydroxide or oxide, and water accounts for that to react the mass percent of total material be 60～90%, M
Oxide or the Average Particle Diameters of hydroxide be 200nm～200 μm；
E the desired amount of Fatty alcohol polyoxyethylene polyoxypropylene ether sulfonate, nonionic surfactant, anionic surface are lived by ()
Property agent, You Heshui be sequentially added in reaction bulb, being warming up to 30～80 DEG C stirs 1～4 hour, obtains required compounding oil base emulsifying
Agent；In terms of mass fraction, Fatty alcohol polyoxyethylene polyoxypropylene ether sulfonate, nonionic surfactant, anionic surface are lived
The proportioning of property agent, oil and water is 0.5～6 part: 0.5～5 part: 0.1～3 part: 5～50 parts: 0.5～1 part.
Fatty alcohol polyoxyethylene poly-oxygen propylene aether sulfonate the most according to claim 7 compounds the preparation of oil base emulsifying agent
Method, it is characterised in that the range of reaction temperature in (a) step is 120～160 DEG C, pressure limit is 0.30～0.60MPa table
Pressure；Fatty alcohol and oxirane, the mol ratio of expoxy propane are 1: 1～5: 5～35, and catalyst amount is fatty alcohol quality
2.5～5.0%；In (b) step the mol ratio of Fatty alcohol polyoxyethylene polyoxypropylene ether, thionyl chloride and pyridine be 1: 1.5～
2.5: 1～2, reaction temperature is 75～90 DEG C, and the response time is 4～8 hours；C in () step, chloro fat alcohol polyoxyethylene gathers
Oxypropylene ether is 1: 1.5～2 with the mol ratio of sulfonated reagent, and 1,3-PD consumption is the 5～8% of reactant quality, and water is used
Amount is the 10～15% of reactant quality, and reaction temperature is 110～140 DEG C, and the response time is 4～8 hours；Fat in (d) step
Fat alcohol polyoxyethylene poly-oxygen propylene aether sulfonic acid is 1.8～2.5: 1 with the oxide of M or the mol ratio of hydroxide, and water accounts for reaction
The mass percent of total material is 70～85%, and the oxide of M or the Average Particle Diameters of hydroxide are 400nm～100 μm,
Reaction temperature is 60～90 DEG C, and the response time is 1～3 hour；(e) in terms of mass fraction, aliphatic alcohol polyethenoxy polyoxypropylene
The amount ranges of ether sulfonate is 1～4 part, and the amount ranges of nonionic surfactant is 1～4 part, anion surface active
The amount ranges of agent is 0.5～1 part, and the amount ranges of oil is 10～40 parts, and the amount ranges of water is 0.5～0.7 part, reaction temperature
Degree is 40～70 DEG C, and mixing time is 2～3 hours.
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| CN1778862A (en) * | 2004-11-17 | 2006-05-31 | 中国石油化工股份有限公司 | Inspissated oil emulsion viscidity reducer |
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