CN110054729A - A kind of oil film dispersin polymerization gel particle transfer drive blocking agent and its synthesis technology - Google Patents
A kind of oil film dispersin polymerization gel particle transfer drive blocking agent and its synthesis technology Download PDFInfo
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- CN110054729A CN110054729A CN201910497939.6A CN201910497939A CN110054729A CN 110054729 A CN110054729 A CN 110054729A CN 201910497939 A CN201910497939 A CN 201910497939A CN 110054729 A CN110054729 A CN 110054729A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/52—Amides or imides
- C08F220/54—Amides, e.g. N,N-dimethylacrylamide or N-isopropylacrylamide
- C08F220/56—Acrylamide; Methacrylamide
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K8/00—Compositions for drilling of boreholes or wells; Compositions for treating boreholes or wells, e.g. for completion or for remedial operations
- C09K8/50—Compositions for plastering borehole walls, i.e. compositions for temporary consolidation of borehole walls
- C09K8/504—Compositions based on water or polar solvents
- C09K8/506—Compositions based on water or polar solvents containing organic compounds
- C09K8/508—Compositions based on water or polar solvents containing organic compounds macromolecular compounds
- C09K8/512—Compositions based on water or polar solvents containing organic compounds macromolecular compounds containing cross-linking agents
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K8/00—Compositions for drilling of boreholes or wells; Compositions for treating boreholes or wells, e.g. for completion or for remedial operations
- C09K8/60—Compositions for stimulating production by acting on the underground formation
- C09K8/84—Compositions based on water or polar solvents
- C09K8/86—Compositions based on water or polar solvents containing organic compounds
- C09K8/88—Compositions based on water or polar solvents containing organic compounds macromolecular compounds
- C09K8/887—Compositions based on water or polar solvents containing organic compounds macromolecular compounds containing cross-linking agents
Abstract
The invention discloses a kind of oil film dispersin polymerization gel particle transfer drive blocking agent and its synthesis technologies.Acrylamide, sodium acrylate, function monomer and deionized water are added first in reaction unit and is configured to monomer mixed aqueous solution, crosslinking agent is added after adjustment pH value, initiator is polymerize.When polymerization reaction reaches accelerated period, monomer mixed aqueous solution can become the non-newtonian fluid of semigel state, carry out draftability cutting using non-newtonian fluid of the stirring involve power to semigel state.The gel particle of cutting is covered with oil film with oil film dispersing agent, avoid between stick to each other.Then it stirs at low speed and continues polymerization reaction under state, reaction temperature, which rises to 80~90 DEG C of reactions, to be terminated.Dilution oil film dispersing agent is added and forms solid-liquid mixed phase, different-grain diameter finished product is then screened out by solid-liquid separation sieve, and recycle oil film dispersing agent.The present invention is novel gel particle synthesis technology, and safety and environmental protection greatly reduces the dosage of oil and surfactant.
Description
Technical field
The invention belongs to oil field profile control agent technical fields, and in particular to a kind of oil film dispersin polymerization gel particle transfer drive is stifled
Agent and its synthesis technology.
Background technique
With world economy and industrial expansion, the mankind are also growing to the demand of petroleum.Due to recent decades pair
The large-scale concentrated extracting of petroleum, geology reservoir is good, the lower oil field block of cost of winning has been approached exhaustion, many oil fields
High, superelevation Water-cut Period is entered, development efficiency is low, and cost of winning is high, and reservoir condition is poor, and heterogeneity is serious.At present due to
New energy can't replace traditional energy completely, so the oil field of some reservoir conditions difference, as Middle East reservoir layer permeability from
0.001 to 5 darcies, infiltration is very poor big, causes recovery ratio low, only reaches 35% or so.And the oil fields such as northern Shensi permeability is extremely low, opens
It is big to adopt difficulty, production efficiency is low, needs to exploit by the methods of pressure break, there are problems that crack channelling.These oil fields have closely
70% crude oil is detained underground, causes resources loss.Want raising recovery ratio to need with technological means such as polymer, gel particles
Big seepage channel is blocked, the crude oil of less permeable layer in starting.Traditional profile control majority is using polymeric material and hands over
Join agent proportion and inject stratum at solution, cross-link intensity control is bad, and be easy to cause hypotonic channel blockage, cannot effectively reach
The purpose of profile control.The problem of improving in terms of products application produced by the invention compared with small particle tradition blocking agent difficulties in dispersion, significantly
It improves the working efficiency of profile control agent application in EOR application and is effectively reduced production cost, therefore be one very significant
Invention.
Dry powder gellike particle transfer drive blocking agent production technology is complicated, and equipment investment is big, and technique is cumbersome, later period dries pulverizing
Equipment input cost and energy loss are big, and the lesser particle of partial size extremely difficult recycling when crushing and screening, easily cause dust pollution.
The innovation of the invention consists in that Novel synthesis technology method is simple, technological equipment investment is few, novel process prevent dust pollution and
By-product compares traditional handicraft, greatly reduces production cost.
Emulsion-type gel particle transfer drive blocking agent effective content is low, and for general effective content in 30-40%, remaining is oil and surface
Activating agent, oil and surfactant largely inject stratum and can cause irreversible membrane fouling to stratum.The innovation of the invention consists in that new
Using the non-newtonian fluid principle of high molecular material, cooperation physics involves shearing force and oil film dispersing agent prepares gel particle transfer drive
Blocking agent, effective content are greater than 95%, and technique later period oil film dispersing agent recycles and reuses, and reduce the dosage of surfactant,
The strong effective pollution reduced to stratum.
Summary of the invention
The purpose of the present invention is to provide a kind of oil film dispersin polymerization gel particle transfer drive blocking agent and its synthesis technologies.
Based on above-mentioned purpose, the present invention is adopted the following technical scheme that:
A kind of oil film dispersin polymerization gel particle transfer drive blocking agent synthesis technology, includes the following steps:
(1) monomer mixed aqueous solution is prepared
Acrylamide, sodium acrylate, function monomer and deionized water are sequentially added in reaction unit, and to be configured to monomer mixed
Heshui solution makes the 30~45wt% of concentration of three kinds of compounds, is adjusted after pH value is 5~8 in stirring and crosslinking agent is added；Wherein
The molar content ratio of acrylamide monomer, sodium acrylate, function monomer is (0.1~0.9): (0.1~0.9): (0.01~
0.2)；
(2) 8-12 DEG C of reaction unit temperature is controlled, nitrogen deoxygenation is then passed to, until being added after oxygen content < 0.1mg/L
Sodium hydrogensulfite is added after being spaced 5~10min in potassium sulfate, continue logical nitrogen to solution it is thick after stop logical nitrogen it is static into
Row polymerization reaction；
(3) it after polymeric reaction temperature rises to 27-31 DEG C, opens stirring while 1~3% oil film dispersing agent is added, to temperature
38-40 DEG C is risen to, stirs at low speed continuation polymerization reaction, but temperature rises to 80-90 DEG C of reaction and terminates；
(4) after reaction, with the poidometer of reactant in reaction unit, 50~80% are added again to diluted oil
Film dispersing agent, and it is cooled to 40-50 DEG C, it is then screened out by separation of solid and liquid screening plant and does not plant size finish product, and oil recovery
Film dispersing agent.
Further, the function monomer is 2- acrylamide-2-methylpro panesulfonic acid (AMPS), N- isopropyl acrylamide
Amine or N- ethyl acrylamide.
Further, adjust in the step (1) pH using it is any in acrylic acid, sodium hydroxide and potassium hydroxide or its
Solution.
Further, the crosslinking agent is methylene diacrylamide, three acrylic acid propane front three alcohol esters or polyethylene glycol two
Acrylate, additional amount be acrylamide, sodium acrylate, function monomer three's gross mass 3%.
Further, the oil film dispersing agent is greater than 200 DEG C of mineral oil and surfactant HLB value less than 5 by boiling point
Compound lipophilic surfactant is made.
Further, the oil film dispersing agent is made of 90-97 parts of mineral oil and 3-10 parts of sapns, detailed process are as follows: will
Mineral oil stirring is warming up to 60-65 DEG C, and sapn is then added, obtains oil film dispersing agent within insulated and stirred 100~150 minutes.
Further, the additional amount of the potassium peroxydisulfate is acrylamide, sodium acrylate, function monomer three's gross mass
0.02%, the additional amount of the sodium hydrogensulfite be acrylamide, sodium acrylate, function monomer three's gross mass 0.03%.
Further, the frequency of blender is 30~50Hz, stirring rate 60- when opening stirring in the step (3)
100rpm rises to 38-40 DEG C to temperature, and the frequency for adjusting blender is 20Hz, and stirring rate is that 40rpm is stirred at low speed.
The oil film dispersin polymerization gel particle transfer drive blocking agent that above-mentioned synthesis technology obtains.
The structural formula of oil film dispersin polymerization gel particle transfer drive blocking agent produced by the present invention is as follows:
In formula R be ethyl, isopropyl orIt is main to improve strand rigidity and temperature sensitivity, to improve
Effective and stability during profile control.
The present invention is special using the non-newtonian fluid of high-molecular gel by the accelerated period at macromolecular polymerization reaction initial stage
Property, cooperate the dispersing method of physics involve power shearing oil film isolation, the gel particle of cutting be covered with oil film with oil film dispersing agent,
Stick to each other between avoiding synthesizes oil film dispersin polymerization gel particle transfer drive blocking agent.
The present invention provides a kind of preparation method of oil film dispersing agent, which stablizes, can after recycling
Reuse does not need to handle, and reduces raw materials for production cost.And adjustable proportion of surfactant controls hydrophobicity, is produced with controlling
The aquation period of product and application effect.
Sieve in the present invention uses stainless steel web plate or stainless (steel) wire, and aperture is required according to product specification, from top to bottom
900-100 microns of sieve plate can be used in the descending arrangement in aperture, aperture.
The present invention is novel gel particle synthesis technology, and safety and environmental protection is stifled compared to traditional dry powder gellike particle transfer drive
Agent, the lesser particle of partial size extremely difficult recycling when crushing and sieving, easily causes dust pollution, stifled compared to emulsion-type gel particle transfer drive
Agent effective content increases by 1 times, greatly reduces the dosage of oil and surfactant, has saved cost and has reduced oily living with surface
The formation contaminant of property agent.
Detailed description of the invention
Fig. 1 is screening plant structural schematic diagram of the present invention, in Fig. 1: 1. solid-liquid mixed phase entrances, and 2. recycle oil film dispersing agents
Outlet, 3. level-ones are separated by solid-liquid separation sieve, and 4. second levels are separated by solid-liquid separation sieve, and 5. three-levels are separated by solid-liquid separation sieve, 6/7. high-frequency vibration dress
It sets, 8/9/10. second level equipment for separating liquid from solid, 11/12/13. secondary recovery oil film dispersant outlet, 14/15/16. gel particle
Transfer drive blocking agent product outlet；
Fig. 2 is non-Newtonian shear of the present invention and dispersion process schematic diagram；
Fig. 3 is the relational graph of different stirring frequencies and particle diameter distribution in embodiment 1 to 4；
Fig. 4 is that oil film dispersant surfactants dosage of the present invention changes to the variation of gel particle transfer drive blocking agent hydration time
Tendency chart；
Fig. 5 is relational graph of 7 to 10 sodium carboxylate groups of embodiment to aquation partial size expansion multiple.
Specific embodiment
In order to keep technical purpose of the invention, technical scheme and beneficial effects clearer, with reference to the accompanying drawing and specifically
Embodiment is further illustrated technical solution of the present invention.
Embodiment 1
A kind of oil film dispersin polymerization gel particle transfer drive blocking agent synthesis technology, steps are as follows:
(1) preparation of oil film dispersing agent
4000 kilograms of mineral oil are added in 5 tons of oily phase kettle, opens stirring heat exchanging interlayer and is passed through steam for mineral oil liter
Warm 60-65 DEG C, 123.7 kilograms of sapn are then added, is controlled 60-65 DEG C of insulated and stirred of temperature 120 minutes, heat exchanging interlayer is passed through cold
But water cooling is spare less than 30 DEG C.
(2) preparation of sodium acrylate
259.3 kilograms and 6.13 kilograms of deionized water of acrylic acid are added in 2 tons and in kettle, opens stirring heat exchanging interlayer
It is passed through refrigerant acrylic acid cools down less than 20 DEG C, is then slowly added into totally 411.3 kilograms of liquid alkaline of 35wt%, continued down control
Neutralization temperature is added as temperature is greater than 30 DEG C of pause liquid alkaline less than 30 DEG C, prevents high temperature autohemagglutination, be finally configured to concentration 50wt%
Sodium acrylate solution it is spare.
(3) monomer mixed aqueous solution is prepared
Using n-isopropyl acrylamide as function monomer, acrylamide monomer, sodium acrylate, the molar content of function monomer
Than for 0.53:0.42:0.05；961.7 kilograms of deionized water are added in 5 tons of reaction unit, is then turned on stirring and successively adds
Enter 326.9 kilograms of acrylamide, 676.8 kilograms of sodium acrylate solution, 34.7 kilograms of function monomer be configured to monomer mixing it is water-soluble
Liquid, it is that first is added in 5 (being adjusted as needed with acrylic acid, sodium hydroxide or potassium hydroxide, similarly hereinafter) afterwards that pH value is adjusted in stirring
21 kilograms of bisacrylamide of fork；Then refrigerant circulation controls 8 DEG C of monomer mixed aqueous solution temperature.Nitrogen deoxygenation is then passed to, until
After oxygen content < 0.1mg/L, it is added 0.14 kilogram of potassium peroxydisulfate, logical nitrogen is continued at interval 5 minutes plus 0.21 kilogram of sodium hydrogensulfite
Gas to solution it is thick after, stop the logical static polymerization reaction of nitrogen, polymeric reaction temperature rises to 27 DEG C of accelerated periods, and unlatching is stirred
It mixes, controls frequency conversion blender 50Hz, stirring rate 100rpm, while being added 30 kilograms of oil film dispersing agent and rising to 38 DEG C of changes to temperature
Frequency blender is adjusted to 20Hz, stirring rate 40rpm, and minuent stirring continues polymerization reaction, as shown in Fig. 2, being high molecular polymerization
Initial reaction stage colloid deformability is stronger, using the non-Newton fluid characteristic of high-molecular gel, cooperates the stretching of physics involve power
Dispersion process, macromolecular polymerization reaction initial stage colloid deformability is stronger, using the non-Newton fluid characteristic of high-molecular gel, matches
The stretching dispersion process of physics involve power is closed, (1) colloid stretches A-stage colloid and is stretched as band-like signal by monolith, (2) glue
Body stretches interim status and is stretched as linear signal by band dress, and (3) colloid stretches later period traditional thread binding close on and is broken signal, and (4) tree lace is disconnected
It splits for graininess signal.To the end of temperature rises to 80 DEG C of reactions, after reaction, the oil film to play diluting effect is added again
1500 kilograms of formation solid-liquid mixed phases of dispersing agent open refrigerant and are cooled to 40 DEG C, then by being separated by solid-liquid separation screening as shown in Figure 1
Device screens out 100-200 μm of partial size, 200-300 μm, 300-500 μm of gel particle transfer drive blocking agent finished product, as shown in Figure 1,
Detailed process is as follows: solid-liquid mixed phase is entered by solid-liquid mixed phase entrance 1 is separated by solid-liquid separation screening plant, solid-liquid separation sieve packing
It sets and is set relatively on the outer wall at middle part there are two dither 6 and 7, solid-liquid mixed phase passes through level-one and is separated by solid-liquid separation the entrance of sieve 3
Second level is separated by solid-liquid separation sieve 4, and the oversize that level-one is separated by solid-liquid separation sieve 3 passes through second level equipment for separating liquid from solid 8 for oil film dispersing agent
It is separated with gel particle transfer drive blocking agent finished product, oil film dispersing agent is isolated and recycled by secondary recovery oil film dispersant outlet 11
It utilizes, 300-500 μm of gel particle transfer drive blocking agent finished product is isolated by gel particle transfer drive blocking agent product outlet 14, is passed through
The solid-liquid mixed phase that second level is separated by solid-liquid separation sieve 4 enters three-level and is separated by solid-liquid separation sieve 5, and second level is separated by solid-liquid separation the oversize of sieve 4
Oil film dispersing agent and gel particle transfer drive blocking agent finished product are separated by second level equipment for separating liquid from solid 9, oil film dispersing agent passes through two
Grade recycling oil film dispersant outlet 12 is isolated and is recycled, and 200-300 μm of gel particle transfer drive blocking agent finished product passes through solidifying
Glue particle transfer drive blocking agent product outlet 15 is isolated, and passes through recycling oil film by the oil film dispersing agent that three-level is separated by solid-liquid separation sieve 5
Dispersant outlet is recovered, and the oversize that three-level is separated by solid-liquid separation sieve 5 passes through second level equipment for separating liquid from solid 10 for oil film dispersing agent
It is separated with gel particle transfer drive blocking agent finished product, oil film dispersing agent is isolated and recycled by secondary recovery oil film dispersant outlet 13
It utilizes, 100-200 μm of gel particle transfer drive blocking agent finished product is isolated by gel particle transfer drive blocking agent product outlet 16.
Gel particle transfer drive blocking agent effective content 96.54% is calculated to obtain by mass ratio, finished product is distributed as 100-200 μm and accounts for
65.4%；200-300 μm accounts for 32.8%；300-500 μm accounts for 1.8%.
The application influence hydrophilic on transfer drive blocking agent on the activity value of oil film dispersing agent is tested, and is as a result detailed in figure
4, as shown in Figure 4, as surfactant is promoted in oil film dispersing agent, hydration time is elongated, illustrates to reduce gel particle tune
The hydrophily of blocking agent is driven, it can be by adjusting the dosage of oil film dispersing agent to adjust the hydration time that different transfer drives block up section.
Embodiment 2
A kind of oil film dispersin polymerization gel particle transfer drive blocking agent synthesis technology, steps are as follows:
(1) oil film dispersing agent recovered liquid is reused；
(2) preparation of sodium acrylate is the same as embodiment 1；
(3) monomer mixed aqueous solution is prepared
Using N- ethyl acrylamide as function monomer, 961.6 kilograms of deionized water are added in 5 tons of reaction unit, so
Afterwards open stirring sequentially add 326.9 kilograms of acrylamide, 676.8 kilograms of sodium acrylate solution, 34.7 kilograms of function monomer and
It is configured to monomer mixed aqueous solution, is adjusted in stirring after pH value is 7 and is added 21 kilograms of methylene diacrylamide, then refrigerant circulation
Control 10 DEG C of monomer mixed aqueous solution temperature.Nitrogen deoxygenation is then passed to, until potassium peroxydisulfate is added after oxygen content < 0.1mg/L
0.14 kilogram, it is static to the thick rear logical nitrogen of stopping of solution to continue logical nitrogen for interval 5 minutes plus 0.21 kilogram of sodium hydrogensulfite
Polymerization reaction, polymeric reaction temperature rise to 28 DEG C of accelerated periods, open stirring, control frequency conversion blender 45Hz, stirring rate
80rpm, while being added 30 kilograms of oil film dispersing agent and rise to 40 DEG C of frequency conversion blenders to temperature and being adjusted to 20Hz, stirring rate
The stirring of 40rpm minuent continues polymerization reaction, to the end of temperature rises to 90 DEG C of reactions, after reaction, dilution oil is added again
1500 kilograms of formation solid-liquid mixed phases of film dispersing agent open refrigerant and are cooled to 45 DEG C, then by being separated by solid-liquid separation screening shown in Fig. 1
Device screens out 100-200 μm of partial size, 200-300 μm, 300-500 μm of gel particle transfer drive blocking agent finished product, passes through mass ratio
Gel particle transfer drive blocking agent effective content 96.65% is calculated to obtain, finished product is distributed as 100-200 μm 55.4%；200-300μm
28.8%；300-500 μm 15.8%.
Embodiment 3
A kind of oil film dispersin polymerization gel particle transfer drive blocking agent synthesis technology, steps are as follows:
(1) oil film dispersing agent recovered liquid is reused；
(2) preparation of sodium acrylate is the same as embodiment 1；
(3) monomer mixed aqueous solution is prepared
Using 2- Methacrylamide -2- methyl propane sulfonic acid sodium as function monomer, deionization is added in 5 tons of reaction unit
It 961.7 kilograms of water, is then turned on stirring and sequentially adds 326.9 kilograms of acrylamide, 676.8 kilograms of sodium acrylate solution, function
34.7 kilograms of monomer and it is configured to monomer mixed aqueous solution, adjusts that methylene diacrylamide 21 is added after pH value is 6 is public in stirring
Jin, then refrigerant circulation controls 12 DEG C of monomer mixed aqueous solution temperature.Nitrogen deoxygenation is then passed to, until oxygen content < 0.1mg/L
Afterwards, it is added 0.14 kilogram of potassium peroxydisulfate, it is thick to solution to continue logical nitrogen for interval 5 minutes plus 0.21 kilogram of sodium hydrogensulfite
Stop the logical static polymerization reaction of nitrogen afterwards, polymeric reaction temperature rises to 31 DEG C of accelerated periods, opens stirring, control frequency conversion stirring
Device 40Hz, stirring rate 70rpm, while being added 30 kilograms of oil film dispersing agent and rise to 40 DEG C of frequency conversion blenders to temperature and being adjusted to
20Hz, the stirring of stirring rate 40rpm minuent continue polymerization reaction, to the end of temperature rises to 85 DEG C of reactions, after reaction, again
Dilution 1500 kilograms of formation solid-liquid mixed phases of oil film dispersing agent are added, opens refrigerant and is cooled to 50 DEG C, it is then logical as shown in Figure 1
Cross be separated by solid-liquid separation screening plant screen out 100-200 μm of partial size, 200-300 μm, 300-500 μm of gel particle transfer drive blocking agent at
Product calculate to obtain gel particle transfer drive blocking agent effective content 95.89% by mass ratio, and finished product is distributed as 100-200 μm 46%；
200-300 μm 23%；300-500 μm 31%.
Embodiment 4
A kind of oil film dispersin polymerization gel particle transfer drive blocking agent synthesis technology, steps are as follows:
(1) oil film dispersing agent recovered liquid is reused；
(2) preparation of sodium acrylate is the same as embodiment 1；
(3) monomer mixed aqueous solution is prepared
Using n-isopropyl acrylamide as function monomer, 961.7 kilograms of deionized water are added in 5 tons of reaction unit,
It is then turned on stirring and sequentially adds 326.9 kilograms of acrylamide, 676.8 kilograms of sodium acrylate solution, 34.7 kilograms of function monomer
Be configured to monomer mixed aqueous solution, adjusted in stirring after pH value is 8 and 21 kilograms of alcohol ester of three acrylic acid propane front three be added, then
Refrigerant circulation controls 10 DEG C of monomer mixed aqueous solution temperature.Nitrogen deoxygenation is then passed to, until being added after oxygen content < 0.1mg/L
0.14 kilogram of potassium peroxydisulfate, it is logical to the thick rear stopping of solution to continue logical nitrogen for interval 5 minutes plus 0.21 kilogram of sodium hydrogensulfite
The static polymerization reaction of nitrogen, polymeric reaction temperature rise to 30 DEG C of accelerated periods, open and stir, control frequency conversion blender 35Hz,
Stirring rate 60rpm, while 30 kilograms of oil film dispersing agent is added rises to 39 DEG C of frequency conversion blenders to temperature and being adjusted to 20Hz, stirring
Rate is that the stirring of 40rpm minuent continues polymerization reaction, to the end of temperature rises to 90 DEG C of reactions, after reaction, is added again dilute
It releases and uses 1500 kilograms of formation solid-liquid mixed phases of oil film dispersing agent, open refrigerant and be cooled to 50 DEG C, then pass through solid-liquid as shown in Figure 1
Separation screening plant screens out 100-200 μm of partial size, 200-300 μm, 300-500 μm of gel particle transfer drive blocking agent finished product, leads to
It crosses mass ratio and calculates to obtain gel particle transfer drive blocking agent effective content 96.32%, finished product is distributed as 100-200 μm 25.4%；200-
300 μm 16.1%；300-500 μm 58.5%.
Influence of the application to the different stirring frequencies of embodiment 1 to 4 to transfer drive blocking agent particle diameter distribution is tested, as a result
It is detailed in Fig. 3.Frequency shown in Fig. 3 is down to 35Hz by 50Hz, and gel particle distribution is occupied an leading position by 100-200 μm of partial size gradually to be become
It occupies an leading position for 300~500 μm of partial sizes, illustrates that speed-frequency has a major impact partial size.
Embodiment 5
A kind of oil film dispersin polymerization gel particle transfer drive blocking agent synthesis technology, steps are as follows:
(1) preparation of oil film dispersing agent
4000 kilograms of mineral oil are added in 5 tons of oily phase kettle, opens stirring heat exchanging interlayer and is passed through steam for mineral oil liter
Warm 60-65 DEG C, 210.5 kilograms of sapn are then added, is controlled 60-65 degrees Celsius of insulated and stirred of temperature 120 minutes, heat exchanging interlayer is logical
It is spare less than 30 DEG C to enter cooling water temperature.
(2) preparation of sodium acrylate is the same as embodiment 1；
(3) monomer mixed aqueous solution is prepared
Using N- ethyl acrylamide as function monomer, 961.7 kilograms of deionized water are added in 5 tons of reaction unit, so
Afterwards open stirring sequentially add 326.9 kilograms of acrylamide, 676.8 kilograms of sodium acrylate solution, 34.7 kilograms of function monomer and
It is configured to monomer mixed aqueous solution, is adjusted in stirring after pH value is 7 and is added 21 kilograms of methylene diacrylamide, it is mixed to be configured to monomer
Heshui solution；Then refrigerant circulation controls 9 DEG C of monomer mixed aqueous solution temperature.Nitrogen deoxygenation is then passed to, until oxygen content <
After 0.1mg/L, it is added 0.14 kilogram of potassium peroxydisulfate, logical nitrogen is continued to solution in interval 5 minutes plus 0.21 kilogram of sodium hydrogensulfite
Stop the logical static polymerization reaction of nitrogen after thick, polymeric reaction temperature rises to 28 DEG C of accelerated periods, opens stirring, and control becomes
Frequency blender 50Hz, stirring rate 100rpm, while 30 kilograms of oil film dispersing agent are added, 40 DEG C of frequency conversion blenders are risen to temperature
It is adjusted to 20Hz, stirring rate 40rpm minuent stirring continuation polymerization reaction, to the end of temperature rises to 85 DEG C of reactions, reaction terminates
Afterwards, dilution 1500 kilograms of formation solid-liquid mixed phases of oil film dispersing agent are added again, opens refrigerant and is cooled to 50 DEG C, then pass through
It is separated by solid-liquid separation screening plant as shown in Figure 1 and screens out 100-200 μm of partial size, 200-300 μm, 300-500 μm of gel particle tune
Blocking agent finished product is driven, gel particle transfer drive blocking agent effective content 96.88% is calculated to obtain by mass ratio.
Embodiment 6
A kind of oil film dispersin polymerization gel particle transfer drive blocking agent synthesis technology, steps are as follows:
(1) preparation of oil film dispersing agent
4000 kilograms of mineral oil are added in 5 tons of oily phase kettle, opens stirring heat exchanging interlayer and is passed through steam for mineral oil liter
Warm 60-65 DEG C, 301.1 kilograms of sapn are then added, is controlled 60-65 DEG C of insulated and stirred of temperature 120 minutes, heat exchanging interlayer is passed through cold
But water cooling is spare less than 30 DEG C.
(2) preparation of sodium acrylate is the same as embodiment 1
(3) monomer mixed aqueous solution is prepared
Using 2- Methacrylamide -2- methyl propane sulfonic acid sodium as function monomer, deionization is added in 5 tons of reaction unit
It 961.7 kilograms of water, is then turned on stirring and sequentially adds 326.9 kilograms of acrylamide, 676.8 kilograms of sodium acrylate solution, function
34.7 kilograms of monomer and it is configured to monomer mixed aqueous solution, adjusts that methylene diacrylamide 21 is added after pH value is 7 is public in stirring
Jin, then refrigerant circulation controls 12 DEG C of monomer mixed aqueous solution temperature.Nitrogen deoxygenation is then passed to, until oxygen content < 0.1mg/L
Afterwards, it is added 0.14 kilogram of potassium peroxydisulfate, it is thick to solution to continue logical nitrogen for interval 5 minutes plus 0.21 kilogram of sodium hydrogensulfite
Stop the logical static polymerization reaction of nitrogen afterwards, polymeric reaction temperature rises to 31 DEG C of accelerated periods, opens stirring, control frequency conversion stirring
Device 50Hz, stirring rate 100rpm are added 30 kilograms of oil film dispersing agent simultaneously, rise to 40 DEG C of frequency conversion blenders to temperature and are adjusted to
20Hz, the stirring of stirring rate 40rpm minuent continue polymerization reaction, to the end of temperature rises to 90 DEG C of reactions, after reaction, again
Dilution 1500 kilograms of formation solid-liquid mixed phases of oil film dispersing agent are added, opens refrigerant and is cooled to 50 DEG C, then by such as Fig. 1 institute
Show be separated by solid-liquid separation screening plant screen out 100-200 μm of partial size, 200-300 μm, 300-500 μm of gel particle transfer drive blocking agent at
Product calculate to obtain gel particle transfer drive blocking agent effective content 96.26% by mass ratio.
Embodiment 7
A kind of oil film dispersin polymerization gel particle transfer drive blocking agent synthesis technology, steps are as follows:
(1) preparation of oil film dispersing agent
4000 kilograms of mineral oil are added in 5 tons of oily phase kettle, opens stirring heat exchanging interlayer and is passed through steam for mineral oil liter
Warm 60-65 DEG C, 395.6 kilograms of sapn are then added, is controlled 60-65 degrees Celsius of insulated and stirred of temperature 120 minutes, heat exchanging interlayer is logical
It is spare less than 30 DEG C to enter cooling water temperature.
(2) preparation of sodium acrylate is the same as embodiment 1；
(3) monomer mixed aqueous solution is prepared
Using n-isopropyl acrylamide as function monomer, 961.7 kilograms of deionized water are added in 5 tons of reaction unit,
It is then turned on stirring and sequentially adds 326.9 kilograms of acrylamide, 676.8 kilograms of sodium acrylate solution, 34.7 kilograms of function monomer
Be configured to monomer mixed aqueous solution, the molar content ratio of acrylamide monomer, sodium acrylate, function monomer is 0.55:0.43:
0.02, it adjusts in stirring after pH value is 5 and is added 21 kilograms of methylene diacrylamide, then the mixing of refrigerant circulation control monomer is water-soluble
8 DEG C of liquid temperature.Nitrogen deoxygenation is then passed to, until being added 0.14 kilogram of potassium peroxydisulfate after oxygen content < 0.1mg/L, is spaced 10 points
Clock adds 0.21 kilogram of sodium hydrogensulfite, continues logical nitrogen to the thick rear logical static polymerization reaction of nitrogen of stopping of solution, polymerization is anti-
It answers temperature to rise to 27 DEG C of accelerated periods, opens stirring, oil is added in control frequency conversion blender 50Hz, stirring rate 100rpm simultaneously
30 kilograms of film dispersing agent rises to that 38 DEG C of frequency conversion blenders are adjusted to 20Hz, the stirring of stirring rate 40rpm minuent continues to gather to temperature
Reaction is closed, to the end of temperature rises to 80 DEG C of reactions, after reaction, dilution is added again and is formed with 1500 kilograms of oil film dispersing agent
Solid-liquid mixed phase opens refrigerant and is cooled to 40 DEG C, then screens out partial size 100- by being separated by solid-liquid separation screening plant as shown in Figure 1
200 μm, 200-300 μm, 300-500 μm of gel particle transfer drive blocking agent finished product, by mass ratio calculate gel particle transfer drive is stifled
Agent effective content 96.33%.
Embodiment 8
A kind of oil film dispersin polymerization gel particle transfer drive blocking agent synthesis technology, steps are as follows:
(1) preparation of oil film dispersing agent
4000 kilograms of mineral oil are added in 5 tons of oily phase kettle, opens stirring heat exchanging interlayer and is passed through steam for mineral oil liter
Warm 60-65 DEG C, 123.7 kilograms of sapn are then added, is controlled 60-65 DEG C of insulated and stirred of temperature 120 minutes, heat exchanging interlayer is passed through cold
But water cooling is spare less than 30 DEG C.
(2) preparation of sodium acrylate
335.8 kilograms and 7.9 kilograms of deionized water of acrylic acid are added in 2 tons and in kettle, opens stirring heat exchanging interlayer
It is passed through refrigerant acrylic acid cools down less than 20 DEG C, is then slowly added into totally 532.7 kilograms of liquid alkaline that concentration is 35%, continued down
Neutralization temperature is controlled less than 30 DEG C degrees Celsius, is added as temperature is greater than 30 DEG C of pause liquid alkaline, is prevented high temperature autohemagglutination, be finally configured to
The sodium acrylate solution of concentration 50wt% is spare.
(3) monomer mixed aqueous solution is prepared
Using 2- acrylamide-2-methylpro panesulfonic acid as function monomer, acrylamide monomer, sodium acrylate, function monomer
Molar content ratio be 0.4:0.58:0.02, in 5 tons of reaction unit be added 861.8 kilograms of deionized water, be then turned on and stir
It mixes and sequentially adds 228.4 kilograms of acrylamide, 876.5 kilograms of sodium acrylate solution, 33.3 kilograms of function monomer and be configured to list
Body mixed aqueous solution adjusts in stirring after pH value is 6 and is added 21 kilograms of polyethyleneglycol diacrylate, and then refrigerant circulation controls
10 DEG C of monomer mixed aqueous solution temperature.Nitrogen deoxygenation is then passed to, until potassium peroxydisulfate 0.14 is added after oxygen content < 0.1mg/L
Kilogram, interval 5 minutes plus 0.21 kilogram of sodium hydrogensulfite, continue logical nitrogen to solution it is thick after, it is static poly- to stop logical nitrogen
Reaction is closed, polymeric reaction temperature rises to 28 DEG C of accelerated periods, opens mixing control frequency conversion blender 50Hz, stirring rate
100rpm, which 30 kilograms of oil film dispersing agent are added simultaneously rise to 40 DEG C of frequency conversion blenders to temperature, is adjusted to 20Hz, stirring rate
40rpm, minuent stirring continue polymerization reaction, to the end of temperature rises to 90 DEG C of reactions, after reaction, dilution oil are added again
1500 kilograms of formation solid-liquid mixed phases of film dispersing agent open refrigerant and are cooled to 50 DEG C, then by being separated by solid-liquid separation screening plant sieve
100-200 μm of partial size, 200-300 μm, 300-500 μm of gel particle transfer drive blocking agent finished product are separated, calculates solidifying by mass ratio
Glue particle transfer drive blocking agent effective content 95.84%.
Embodiment 9
A kind of oil film dispersin polymerization gel particle transfer drive blocking agent synthesis technology, steps are as follows:
(1) oil film dispersing agent recovered liquid is reused
(2) preparation of sodium acrylate
283.6 kilograms and 9.1 kilograms of deionized water of acrylic acid are added in 2 tons and in kettle, opens stirring heat exchanging interlayer
It is passed through refrigerant acrylic acid cools down less than 20 DEG C, is then slowly added into totally 608.5 kilograms of liquid alkaline that concentration is 35wt%, it is lasting to drop
Temperature control neutralization temperature is added as temperature is greater than 30 DEG C of pause liquid alkaline less than 30 DEG C degrees Celsius, prevents high temperature autohemagglutination, final to prepare
Sodium acrylate solution at concentration 50wt% is spare.
(3) monomer mixed aqueous solution is prepared
Using n-isopropyl acrylamide as function monomer, acrylamide monomer, sodium acrylate, the molar content of function monomer
Than 799.4 kilograms of deionized water being added in 5 tons of reaction unit, is then turned on stirring and sequentially adds for 0.3:0.68:0.02
166.9 kilograms of acrylamide, 1001.2 kilograms of sodium acrylate solution, 32.4 kilograms of function monomer and be configured to monomer mixing it is water-soluble
Liquid adjusts in stirring after pH value is 6 and 21 kilograms of alcohol ester of three acrylic acid propane front three is added, then the mixing of refrigerant circulation control monomer
12 DEG C of aqueous temperature.Nitrogen deoxygenation is then passed to, until being added 0.14 kilogram of potassium peroxydisulfate, interval after oxygen content < 0.1mg/L
5 minutes plus 0.21 kilogram of sodium hydrogensulfite, continue logical nitrogen to the thick rear logical static polymerization reaction of nitrogen of stopping of solution, polymerization
Reaction temperature rises to 28 DEG C of accelerated periods, opens mixing control frequency conversion blender 50Hz, 800rpm speed and oil film is added simultaneously
30 kilograms of dispersing agent rise to 40 DEG C of frequency conversion blenders to temperature and are adjusted to 20Hz, stirring rate 40rpm, and minuent stirring continues to polymerize
Reaction after reaction, dilution is added again and is formed admittedly with 1500 kilograms of oil film dispersing agent to the end of temperature rises to 90 DEG C of reactions
Liquid mixed phase opens refrigerant and is cooled to 50 DEG C, then screens out partial size 100- by being separated by solid-liquid separation screening plant as shown in Figure 1
200 μm, 200-300 μm, 300-500 μm of gel particle transfer drive blocking agent finished product, by mass ratio calculate gel particle transfer drive is stifled
Agent effective content 96.61%.
Embodiment 10
A kind of oil film dispersin polymerization gel particle transfer drive blocking agent synthesis technology, steps are as follows:
(1) oil film dispersing agent recovered liquid is reused
(2) preparation of sodium acrylate
428.9 kilograms and 10.3 kilograms of deionized water of acrylic acid are added in 2 tons and in kettle, opens stirring heat exchanging interlayer
It is passed through refrigerant acrylic acid cools down less than 20 DEG C, is then slowly added into totally 680.5 kilograms of liquid alkaline that concentration is 35wt%, it is lasting to drop
Temperature control neutralization temperature is added as temperature is greater than 30 DEG C of pause liquid alkaline less than 30 DEG C degrees Celsius, prevents high temperature autohemagglutination, final to prepare
Sodium acrylate solution at concentration 50wt% is spare.
(3) monomer mixed aqueous solution is prepared
Using 2- Methacrylamide -2- methyl propane sulfonic acid sodium as function monomer, acrylamide monomer, sodium acrylate, function
The molar content ratio of monomer is 0.2:0.78:0.02, and 740.1 kilograms of deionized water are added in 5 tons of reaction unit, then opens
Stirring is opened to sequentially add 108.5 kilograms of acrylamide, 1119.7 kilograms of sodium acrylate solution, 31.6 kilograms of function monomer and prepare
At monomer mixed aqueous solution, is adjusted in stirring after pH value is 8 and be added 21 kilograms of methylene diacrylamide, then refrigerant circulation controls
10 DEG C of monomer mixed aqueous solution temperature.Nitrogen deoxygenation is then passed to, until potassium peroxydisulfate 0.14 is added after oxygen content < 0.1mg/L
Kilogram, logical nitrogen is continued to the thick rear logical static polymerization of nitrogen of stopping of solution in interval 5 minutes plus 0.21 kilogram of sodium hydrogensulfite
Reaction, polymeric reaction temperature rise to 31 DEG C of accelerated periods, open stirring, control frequency conversion blender 40Hz, stirring rate 70rpm
Speed, while 30 kilograms of oil film dispersing agent are added, 40 DEG C of frequency conversion blenders, which are risen to, to temperature is adjusted to 20Hz, stirring rate
40rpm, minuent stirring continue polymerization reaction, to the end of temperature rises to 90 DEG C of reactions, after reaction, dilution oil are added again
1500 kilograms of formation solid-liquid mixed phases of film dispersing agent open refrigerant and are cooled to 50 DEG C, then pass through solid-liquid separation sieve as shown in Figure 1
Separating device screens out 100-200 μm of partial size, 200-300 μm, 300-500 μm of gel particle transfer drive blocking agent finished product, passes through quality
Than calculating to obtain gel particle transfer drive blocking agent effective content 96.52%,
Fig. 5 is influence of 7 to the 10 gained transfer drive blocking agent of embodiment to aquation partial size expansion multiple, third in embodiment 7 to 10
Olefin(e) acid sodium accounts for acrylamide respectively, the molar ratio in three kinds of monomers of sodium acrylate and function monomer is respectively 0.43,0.58,
0.68,0.78, as shown in Figure 5, sodium carboxylate groups' content improves in gel particle transfer drive blocking agent, and Bulking Time and expansion multiple are all
It is corresponding to be promoted, show that expansion multiple can be controlled with hydration time.
Claims (9)
1. a kind of oil film dispersin polymerization gel particle transfer drive blocking agent synthesis technology, which is characterized in that include the following steps:
(1) monomer mixed aqueous solution is prepared
Acrylamide, sodium acrylate, function monomer and deionized water are sequentially added in reaction unit is configured to monomer mixing water
Solution makes the 30 ~ 45wt% of concentration of three kinds of compounds, is adjusted after pH value is 5 ~ 8 in stirring and crosslinking agent is added；Wherein acryloyl
Amine monomers, sodium acrylate, the molar content ratio of function monomer are (0.1 ~ 0.9): (0.1 ~ 0.9): (0.01 ~ 0.2)；
(2) 8-12 DEG C of reaction temperature is controlled, nitrogen deoxygenation is then passed to, until potassium peroxydisulfate is added after oxygen content < 0.1mg/L,
Sodium hydrogensulfite is added after being spaced 5 ~ 10min, continues logical nitrogen and polymerize instead to the thick rear logical nitrogen of stopping of solution is static
It answers；
(3) it after polymeric reaction temperature rises to 27-31 DEG C, opens stirring while the 1-3% oil film of polymerization reaction material gross mass is added
Dispersing agent rises to 38-40 DEG C to temperature, stirs at low speed continuation polymerization reaction, but temperature rises to 80-90 DEG C of reaction and terminates；
(4) after reaction, with the poidometer of reactant in reaction unit, 50 ~ 80% is added again and disperses to diluted oil film
Agent, and it is cooled to 40-50 DEG C, it is then screened out by separation of solid and liquid screening plant and does not plant size finish product, and recycle oil film dispersion
Agent.
2. oil film dispersin polymerization gel particle transfer drive blocking agent synthesis technology according to claim 1, which is characterized in that the function
Energy monomer is 2- acrylamide-2-methylpro panesulfonic acid, n-isopropyl acrylamide or N- ethyl acrylamide.
3. oil film dispersin polymerization gel particle transfer drive blocking agent synthesis technology according to claim 1, which is characterized in that the step
Suddenly pH is adjusted in (1) use any or its solution in acrylic acid, sodium hydroxide and potassium hydroxide.
4. oil film dispersin polymerization gel particle transfer drive blocking agent synthesis technology according to claim 1, which is characterized in that the friendship
Connection agent is that methylene diacrylamide, three acrylic acid propane front three alcohol esters or polyethyleneglycol diacrylate, additional amount are acryloyl
Amine, sodium acrylate, function monomer three's gross mass 3%.
5. oil film dispersin polymerization gel particle transfer drive blocking agent synthesis technology according to claim 1, which is characterized in that the oil
Film dispersing agent is greater than the compound lipophilic surfactant system of 200 DEG C of mineral oil and surfactant HLB value less than 5 by boiling point
?.
6. oil film dispersin polymerization gel particle transfer drive blocking agent synthesis technology according to claim 5, which is characterized in that the oil
Film dispersing agent is made of 90-97 parts of mineral oil and 3-10 parts of sapns, detailed process are as follows: mineral oil stirring is warming up to 60-65 DEG C,
Then sapn is added, obtains oil film dispersing agent within insulated and stirred 100 ~ 150 minutes.
7. oil film dispersin polymerization gel particle transfer drive blocking agent synthesis technology according to claim 1, which is characterized in that the mistake
The additional amount of potassium sulfate be acrylamide, sodium acrylate, function monomer three's gross mass 0.02%, the sodium hydrogensulfite
Additional amount be acrylamide, sodium acrylate, function monomer three's gross mass 0.03%.
8. oil film dispersin polymerization gel particle transfer drive blocking agent synthesis technology according to claim 1, which is characterized in that the step
The frequency of blender is 30 ~ 50Hz, stirring rate 60-100rpm when opening stirring in (3) suddenly, rises to 38-40 DEG C to temperature, adjusts
The frequency of whole blender is 20Hz, and stirring rate is that 40rpm is stirred at low speed.
9. the oil film dispersin polymerization gel particle transfer drive blocking agent that any synthesis technology of claim 1 to 8 obtains.
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Citations (3)
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|---|---|---|---|---|
| JP2003514961A (en) * | 1999-11-20 | 2003-04-22 | ビーエーエスエフ アクチェンゲゼルシャフト | Method for continuous production of crosslinked fine-grained gel-like polymer |
| CN102127189A (en) * | 2010-12-24 | 2011-07-20 | 北京石大万嘉新材料科技有限公司 | Polyacrylamide microgel as well as preparation method and application thereof |
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2019
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2003514961A (en) * | 1999-11-20 | 2003-04-22 | ビーエーエスエフ アクチェンゲゼルシャフト | Method for continuous production of crosslinked fine-grained gel-like polymer |
| CN102127189A (en) * | 2010-12-24 | 2011-07-20 | 北京石大万嘉新材料科技有限公司 | Polyacrylamide microgel as well as preparation method and application thereof |
| CN107987211A (en) * | 2017-12-07 | 2018-05-04 | 河南正佳能源环保股份有限公司 | The synthetic method of quarternary copolymerized salt resistance temperature resistance polyacrylamide |
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