CN106833574B - A kind of water-soluble diversion agent and preparation method thereof - Google Patents

A kind of water-soluble diversion agent and preparation method thereof Download PDF

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CN106833574B
CN106833574B CN201611258380.4A CN201611258380A CN106833574B CN 106833574 B CN106833574 B CN 106833574B CN 201611258380 A CN201611258380 A CN 201611258380A CN 106833574 B CN106833574 B CN 106833574B
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water
soluble
straight chain
polylactide
diversion agent
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CN106833574A (en
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耿立涛
任瑞波
徐茜
杨立君
邢万东
李新胜
张利军
张哲�
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QINGDAO KEKAIDA RUBBER PLASTIC CO Ltd
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    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09KMATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K8/00Compositions for drilling of boreholes or wells; Compositions for treating boreholes or wells, e.g. for completion or for remedial operations
    • C09K8/50Compositions for plastering borehole walls, i.e. compositions for temporary consolidation of borehole walls
    • C09K8/504Compositions based on water or polar solvents
    • C09K8/506Compositions based on water or polar solvents containing organic compounds
    • C09K8/508Compositions based on water or polar solvents containing organic compounds macromolecular compounds
    • C09K8/5086Compositions based on water or polar solvents containing organic compounds macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
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    • C08GMACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G63/00Macromolecular compounds obtained by reactions forming a carboxylic ester link in the main chain of the macromolecule
    • C08G63/68Polyesters containing atoms other than carbon, hydrogen and oxygen
    • C08G63/685Polyesters containing atoms other than carbon, hydrogen and oxygen containing nitrogen
    • C08G63/6852Polyesters containing atoms other than carbon, hydrogen and oxygen containing nitrogen derived from hydroxy carboxylic acids
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    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08GMACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G63/00Macromolecular compounds obtained by reactions forming a carboxylic ester link in the main chain of the macromolecule
    • C08G63/68Polyesters containing atoms other than carbon, hydrogen and oxygen
    • C08G63/692Polyesters containing atoms other than carbon, hydrogen and oxygen containing phosphorus
    • C08G63/6922Polyesters containing atoms other than carbon, hydrogen and oxygen containing phosphorus derived from hydroxy carboxylic acids
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    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08GMACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G79/00Macromolecular compounds obtained by reactions forming a linkage containing atoms other than silicon, sulfur, nitrogen, oxygen, and carbon with or without the latter elements in the main chain of the macromolecule
    • C08G79/02Macromolecular compounds obtained by reactions forming a linkage containing atoms other than silicon, sulfur, nitrogen, oxygen, and carbon with or without the latter elements in the main chain of the macromolecule a linkage containing phosphorus
    • C08G79/025Polyphosphazenes
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    • C09K2208/00Aspects relating to compositions of drilling or well treatment fluids
    • C09K2208/10Nanoparticle-containing well treatment fluids
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
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    • C09K2208/00Aspects relating to compositions of drilling or well treatment fluids
    • C09K2208/34Lubricant additives

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Abstract

The present invention relates in oil extraction process fracture stimulation operations and oil recovery technology of reservoir sweep field, and in particular to a kind of water-soluble diversion agent and preparation method thereof.It includes 50~100 parts of straight chain branched polylactide, 5~20 parts of plasticizer, 3~8 parts of nanoreinforcement material that water-soluble diversion agent, which prepares raw material, and 0.1~0.3 part of antioxidant, 0.5~1 part of lubricant.The water-soluble diversion agent the preparation method comprises the following steps: straight chain poly phosphazene is synthesized with polylactide first, available straight chain branched polylactide;Then straight chain branched polylactide, plasticizer, nanoreinforcement material, antioxidant, lubricant are kneaded in mixer in proportion uniform, then pass through extruding pelletization in double screw extruder, through squeezing out tie rod after extruder squeezes out, water cooling, it air-dries, it is granulated and is crushed, prepare the water-soluble diversion agent of different-grain diameter after screening.The water-soluble diversion agent can preferably be dissolved in water, and degrade in water;It, can pressure-bearing 30MPa or more with higher bearing strength.

Description

A kind of water-soluble diversion agent and preparation method thereof
Technical field
The present invention relates in oil extraction process fracture stimulation operations and oil recovery technology of reservoir sweep field, and in particular to it is a kind of Water-soluble diversion agent and preparation method thereof.
Background technique
Pressure break diversion agent is one of oil-water well transformation process auxiliary additive, is called pressure break diverting agent, it is to turn to Important component part in fracturing technique.In pressing crack construction, using the temporarily stifled old seam of the bridge blinding effect of diversion agent or sand is added to stitch, Winding shaft bottom net pressure, turns to fluid in the earth formation, forms the new crack for being different from old fractuer direction or makes fracturing sand It is uniformly distributed in crack, to open new fluid flowing passage in reservoir, more broadly links up old crack and do not employ Oil-gas Layer, increase oil and gas production.Diversion agent used at present mainly has: silicic acid salt grain, haydite, polyacrylamide etc., silicic acid That there are density is big for salt grain, haydite, pumps extremely difficult, low efficiency, insoluble;It is low equal scarce to there is closure pressure in polyacrylamide It falls into.Therefore my company develops that intensity is higher, and solution temperature and speed are controllable, dissolves thoroughly water-soluble diversion agent.
Summary of the invention
Present invention seek to address that the above problem, a kind of water-soluble diversion agent and preparation method thereof is provided, with intensity height, Solution temperature and speed are controllable, dissolve the features such as thorough.The invention is realized by the following technical scheme:
A kind of water-soluble diversion agent, is made of the raw material of parts by weight as shown below:
Material name Component
Straight chain branched polylactide 50~100 parts
Plasticizer 5-20 parts
Nanoreinforcement material 3-8 parts
Antioxidant 0.1-0.3 parts
Lubricant 0.5-1 parts
Straight chain branched polylactide is the highly -branched degree polymer being polymerized by straight chain poly phosphazene and polylactide, preferably Five branched polylactides.Straight chain poly phosphazene is the straight chain phosphine nitrile of the molecular weight that is polymerized by dichloro phosphine nitrile in 200-5000, excellent Select pentachloro- phosphine nitrile.Straight chain poly phosphazene and the reaction equation of polylactide polymerization reaction are
Straight chain branched polylactide is prepared by following methods:
1) phosphine nitrile five is etherified the synthesis of benzaldehyde
10~20 parts of parahydroxyben-zaldehyde of addition in a kettle, 100 parts of solvent, after stirring and dissolving, lower point of nitrogen atmosphere It criticizes and is added 5~30 parts of catalyst, keep 0 DEG C of temperature in kettle, be warmed to room temperature after adding after the reaction was continued 2 hours and be down to -5 DEG C again.By 3 ~10 parts of pentachloro- phosphine nitriles are dissolved in 17 parts of solvents, are warmed to room temperature after being slowly added dropwise in reaction kettle in 1.5 hours at -5 DEG C And it is stirred to react 16 hours.
Pentachloro- phosphine nitrile CAS:13966-08-0, English name: (Dichlorophosphinyl) phosphorimidic Trichloride, molecular weight 269.22.
Reaction solution is filtered after reaction, and elutes filter cake, merging filtrate in three times with 50 parts of solvents, rotation volatilization removes It goes after solvent to recrystallize to obtain the etherificate benzaldehyde of pale yellow crystals intermediate product phosphine nitrile five with normal heptane or dehydrated alcohol, for use.
2) phosphine nitrile five is etherified the synthesis of benzyl alcohol
3~7 parts of reducing agents are dissolved in 20~40 parts of solvent, 2~5 parts of compatilizers are added, are stirred evenly stand-by;By 25 ~30 parts of phosphine nitriles five are etherified benzaldehyde and are dissolved in 100 parts of solvents, are slowly added dropwise in prepared reducing agent solution at 0 DEG C, And it is warmed to room temperature that the reaction was continued 1 hour.It is converted completely by gas-chromatography tracking reaction to aldehyde radical.2~4 are added after reaction Part terminator simultaneously stirs 12 hours.
Solvent is persistently removed to thick, 100~400 parts of the addition into residue using rotation volatilization after stirring 12 hours Extractant extracts intermediate product B, and 10 parts of desiccant dryness are added after stirring 2 hours.It filters and is spin-dried for filtrate and obtain intermediate production Object phosphine nitrile five is etherified benzyl alcohol, for use.
3) synthesis of straight chain branched polylactide
2~2.5 parts of phosphine nitriles five are etherified benzyl alcohol, 0.005~0.007 part of initiator, 5L high pressure is added in 100 parts of lactides It in kettle, can also be added and 0~50 part of auxiliary diluent, being warming up to 180 DEG C after stirring 2 hours at 120 DEG C, the reaction was continued 5 hours Obtain off-white powder product straight chain branched polylactide.
The catalyst is one or more of triethylamine, triisopropylamine, potassium carbonate and sodium hydride;
And/or the solvent is one or more of anhydrous THF or anhydrous propanone;
And/or the preferred sodium borohydride of reducing agent;
And/or the ammonium chloride solution of the terminator preferably 5% concentration;
And/or the auxiliary diluent is one or both of toluene, dimethylbenzene;
And/or the preferred methylene chloride of extractant;
And/or the preferred anhydrous sodium sulfate of desiccant;
And/or the initiator preferably octanoic acid stannous;
And/or the auxiliary diluent is one or more of toluene, dimethylbenzene;
And/or the plasticizer is one of poly-hydroxy fatty acid, PEG, polytrimethylene carbonate PTMC or several Kind;
And/or the nanoreinforcement material be one of nanometer calcium carbonate, Nano carbon white, nanoscale talcum powder or It is several;
And/or the antioxidant is antioxidant 1010, antioxidant 1076, antioxidant 164, antioxidant 264, antioxidant CA One or more of;
The lubricant is one or more of stearic acid, tristerin, paraffin, OPE wax, silicone oil;
A kind of preparation method of water-soluble diversion agent comprising the steps of:
1) by straight chain branched polylactide, plasticizer, nanoreinforcement material, antioxidant, lubricant in proportion in mixer Middle to be kneaded uniformly, mixer temperature control control is at 90~120 DEG C or so, 8~10min of mixing time.
2) then by extruding pelletization in double screw extruder, extrusion temperature is 90~100 DEG C of an area, 2nd area~4th area 110~125 DEG C, 5th area~105~120 DEG C of tenth area, 11 area's temperature are 110 DEG C.Through squeezing out tie rod, water after extruder squeezes out It is cold, it air-dries, is granulated and is crushed, prepare water-soluble diversion agent after screening.
Water-soluble diversion agent prepared by the present invention have a characteristic that 1. have higher bearing strength, can pressure-bearing 30MPa with On;2. solution temperature and dissolution time are adjustable;3. dissolution is thoroughly, without insoluble resin particle;4. diversion agent grain diameter can lead to Broken milling process control is crossed, different pressure break scale requirements can be met.
Specific embodiment
Following part is that the present invention will be further described for specific embodiment, but following implementation is only to this hair Bright is explained further, and does not represent the scope of the present invention and is only limitted to this, all equivalence replacements done with thinking of the invention, In protection scope of the present invention, for explaining only the invention, and it is not considered as limiting the invention.
Embodiment 1
1) phosphine nitrile five is etherified the synthesis of benzaldehyde
Parahydroxyben-zaldehyde 610g, anhydrous THF 3L are added in a kettle, after stirring and dissolving, under nitrogen atmosphere in batches plus Enter sodium hydride 200g (60%), is kept for 0 DEG C of temperature in the kettle, be warmed to room temperature after adding after the reaction was continued 2 hours and be down to -5 DEG C again.Five Chlorine phosphine nitrile 269g is dissolved in the anhydrous THF of 500mL, is warmed to room temperature simultaneously after being slowly added dropwise in reaction kettle in 1.5 hours at -5 DEG C It is stirred to react 16 hours.
Reaction solution is filtered after reaction and filter cake, merging filtrate are eluted in three times with the anhydrous THF of 1L, rotation volatilization removes It goes after solvent to recrystallize to obtain pale yellow crystals 648g with normal heptane or dehydrated alcohol, is etherified benzaldehyde, yield 93% for phosphine nitrile five.
2) phosphine nitrile five is etherified the synthesis of benzyl alcohol
Sodium borohydride 19g is dissolved in 200mLTHF and 10mL alcohol mixeding liquid, obtains sodium borohydride solution, and phosphine nitrile five is etherified benzene Formaldehyde 139.4g is dissolved in 500mL THF, is slowly added dropwise in gained sodium borohydride solution at 0 DEG C and is warmed to room temperature that the reaction was continued 1 hour.GC tracking reaction converts completely to aldehyde radical.
20 milliliters of 5% ammonium chloride solution is added after reaction and stirs 12 hours.
Solvent is persistently removed to thick, the addition 2L dichloromethane into residue using rotation volatilization after stirring 12 hours It is dry that anhydrous sodium sulfate is added after stirring 2 hours in alkane.It filters and is spin-dried for filtrate and obtain dope 139g, be etherified benzene first for phosphine nitrile five Alcohol, yield 98.3%.
3) synthesis of straight chain branched polylactide:
Phosphine nitrile five is etherified benzyl alcohol 70.7g, stannous octoate 0.2g, lactide 3000g, be added in 5L autoclave 120 DEG C it is anti- 180 DEG C are warming up to after answering 2 hours the reaction was continued 5 hours and to obtain off-white powder 3048g, is straight chain branched polylactide, yield 99.3%.
Gained straight chain branched polylactide is five branched polylactides, is detected through GPC:
Mn:22890, Mw/Mn=1.17, Mp:129 DEG C, crystallinity: 20.6%.
4) preparation of Water soluble diversion agent
By 79.2 parts of five branched polylactide, 10 parts of PEG400,10 parts of nanometer calcium carbonate, 0.2 part of antioxidant 1010, resist 264 0.1 parts of oxygen agent, 0.5 part of calcium stearate is put into mixer, mixing 8 minutes at 110 DEG C.Then the good masterbatch of mixing is added Entering extruding pelletization in double screw extruder, extrusion temperature is 100 DEG C of an area, 2nd area~120 DEG C of 4th area, 5th area~110 DEG C of tenth area, 11 110 DEG C of area's temperature.Tie rod is squeezed out after extruder squeezes out, water cooling air-dries, and is granulated, obtains uniformly mixed plastic pellet Son is Water soluble diversion agent.
Embodiment 2
1) phosphine nitrile five is etherified the synthesis of benzaldehyde
It is added parahydroxyben-zaldehyde 610g, triethylamine 606g, anhydrous THF 3L in a kettle, after stirring and dissolving, nitrogen It is added portionwise under atmosphere sodium hydride 200g (60%), is kept for 0 DEG C of temperature in the kettle, be warmed to room temperature after adding after the reaction was continued 2 hours It is down to -5 DEG C again.Pentachloro- phosphine nitrile 269g is dissolved in the anhydrous THF of 500mL, in being slowly added dropwise in reaction kettle in 1.5 hours at -5 DEG C After be warmed to room temperature and be stirred to react 16 hours.
Reaction solution is filtered after reaction and filter cake, merging filtrate are eluted in three times with the anhydrous THF of 1L, rotation volatilization removes It goes after solvent to recrystallize to obtain pale yellow crystals 664g with normal heptane or dehydrated alcohol, is etherified benzaldehyde, yield for phosphine nitrile five 95.2%.HNMR (400M, d6-DMSO): 7.04ppm (d, 2H), 7.78ppm (d, 2H), 9.93ppm (s, 1H).
2) phosphine nitrile five is etherified the synthesis of benzyl alcohol
Sodium borohydride 38g is dissolved in 200mLTHF and 50mL alcohol mixeding liquid, obtains sodium borohydride solution, and phosphine nitrile five is etherified benzene Formaldehyde 278g is dissolved in 1000mL THF and is slowly added dropwise in gained sodium borohydride solution at 0 DEG C and is warmed to room temperature that the reaction was continued 1 Hour.GC tracking reaction converts completely to aldehyde radical.
20 milliliters of 5% ammonium chloride solution is added after reaction and stirs 12 hours.
Solvent is persistently removed to thick, the addition 1.2L dichloromethane into residue using rotation volatilization after stirring 12 hours It is dry that anhydrous sodium sulfate is added after stirring 2 hours in alkane.It filters and is spin-dried for filtrate and obtain dope 282g, be etherified benzene first for phosphine nitrile five Alcohol, yield 100%.
3) synthesis of straight chain branched polylactide:
Phosphine nitrile five is etherified benzyl alcohol 48g, stannous octoate 0.1g, lactide 2000g, and toluene 1000mL is added in 5L autoclave 120 DEG C be warming up to 180 DEG C after reaction 2 hours the reaction was continued 5 hours after solvent be evaporated off obtain off-white powder 2048g, be straight chain branch Change polylactide, yield 100%.
Gained straight chain branched polylactide is five branched polylactides, is detected through GPC:
Mn:24860, Mw/Mn=1.21, Mp:138 DEG C, crystallinity: 21.3%.
4) preparation of Water soluble diversion agent
By 76 parts of five branched polylactide, 15 parts of polyhydroxyalkanoate, 8 parts of Nano carbon white, antioxidant 1010 0.2 Part, 164 0.1 parts of antioxidant, 0.7 part of OPE wax is put into mixer, mixing 8 minutes at 120 DEG C.Then the masterbatch that mixing is good Extruding pelletization is added twin-screw extrude, extrusion temperature is 90 DEG C of an area, 2nd area~115 DEG C of 4th area, 5th area~ten areas 115 DEG C, 11 110 DEG C of area's temperature.Tie rod is squeezed out after extruder squeezes out, water cooling air-dries, and is granulated, obtains uniformly mixed plastics Particle.
Embodiment 3
1) phosphine nitrile five is etherified the synthesis of benzaldehyde
Parahydroxyben-zaldehyde 305g, potassium carbonate 379.5g, anhydrous propanone 3L, after stirring and dissolving, nitrogen are added in a kettle Atmosphere is added portionwise sodium hydride 200g (60%) under enclosing, and is kept for 0 DEG C of temperature in the kettle, is warmed to room temperature that the reaction was continued 2 hours after adding It is down to -5 DEG C again afterwards.Pentachloro- phosphine nitrile 134.5g is dissolved in 500mL anhydrous propanone, anti-in being slowly added dropwise in 1.5 hours at -5 DEG C It is warmed to room temperature and is stirred to react 16 hours after answering in kettle.
Reaction solution is filtered after reaction and filter cake, merging filtrate are eluted in three times with 0.5L anhydrous propanone, rotation is waved Normal heptane/dehydrated alcohol recrystallizes to obtain pale yellow crystals 342g after hair removes solvent, is etherified benzaldehyde, yield for phosphine nitrile five 98.1%.
2) phosphine nitrile five is etherified the synthesis of benzyl alcohol
Sodium borohydride 38g is dissolved in 200mLTHF and 50mL methyl alcohol mixed liquor, and phosphine nitrile five is etherified benzaldehyde 278g and is dissolved in 1000mL THF is slowly added dropwise in gained sodium borohydride solution at 0 DEG C and is warmed to room temperature that the reaction was continued 1 hour.GC tracking is anti- It should be converted completely to aldehyde radical.
20 milliliters of 5% ammonium chloride solution is added after reaction and stirs 12 hours.
Solvent is persistently removed to thick, the addition 1L dichloromethane into residue using rotation volatilization after stirring 12 hours It is dry that anhydrous sodium sulfate is added after stirring 2 hours in alkane.It filters and is spin-dried for filtrate and obtain dope 282g, be etherified benzene first for phosphine nitrile five Alcohol, yield 100%.
3) synthesis of straight chain branched polylactide
Phosphine nitrile five is etherified benzyl alcohol 48g, stannous octoate 0.1g, lactide 2000g, and 5L autoclave is added in dimethylbenzene 500mL In 120 DEG C be warming up to 180 DEG C after 2 hours the reaction was continued 5 hours after solvent be evaporated off obtain off-white powder 2048g, be straight chain branching Polylactide, yield 100%.
Gained straight chain branched polylactide is five branched polylactides, is detected through GPC:
Mn:21495, Mw/Mn=1.32, Mp:126 DEG C, crystallinity: 19.8%.
4) preparation of Water soluble diversion agent
By 64 parts of five branched polylactide, 20 parts of PEG400,15 parts of nano talc, 0.3 part of antioxidant CA, paraffin 0.7 Part is put into mixer, mixing 8 minutes at 100 DEG C.Then the good masterbatch of mixing is added twin-screw extrude into extruding pelletization, Extrusion temperature is 100 DEG C of an area, 2nd area~110 DEG C of 4th area, 5th area~120 DEG C of tenth area, 11 110 DEG C of area's temperature.Through extruder Tie rod is squeezed out after extrusion, water cooling air-dries, and is granulated, obtains uniformly mixed plastic pellet, is Water soluble diversion agent.
Embodiment 4
1) phosphine nitrile five is etherified the synthesis of benzaldehyde
Parahydroxyben-zaldehyde 610g, triisopropylamine 786.5g, anhydrous THF 3L, stirring and dissolving are added in a kettle Afterwards, it is added portionwise under nitrogen atmosphere sodium hydride 200g (60%), is kept for 0 DEG C of temperature in the kettle, be warmed to room temperature that the reaction was continued after adding 2 It is down to -5 DEG C again after hour.Pentachloro- phosphine nitrile 250g is dissolved in the anhydrous THF of 500mL, anti-in being slowly added dropwise in 1.5 hours at -5 DEG C It is warmed to room temperature and is stirred to react 16 hours after answering in kettle.
Reaction solution is filtered after reaction and filter cake, merging filtrate are eluted in three times with the anhydrous THF of 1L, rotation volatilization removes It goes after solvent to recrystallize to obtain pale yellow crystals 639g with normal heptane or dehydrated alcohol, is straight chain phosphine nitrile ether benzaldehyde.
2) phosphine nitrile five is etherified the synthesis of benzyl alcohol
Sodium borohydride 30g is dissolved in 200mLTHF and 10mL alcohol mixeding liquid, and poly phosphazene etherificate benzaldehyde 130g is dissolved in 500mL THF is slowly added dropwise in gained sodium borohydride solution at 0 DEG C and is warmed to room temperature that the reaction was continued 1 hour.GC tracking is reacted to aldehyde Base converts completely.
20 milliliters of 5% ammonium chloride solution is added after reaction and stirs 12 hours.
Solvent is persistently removed to thick, the addition 2L dichloromethane into residue using rotation volatilization after stirring 12 hours It is dry that anhydrous sodium sulfate is added after stirring 2 hours in alkane.It filters and is spin-dried for filtrate and obtain dope 130g, be etherified benzene first for phosphine nitrile five Alcohol, yield 99.1%.
3) synthesis of straight chain branched polylactide
Poly phosphazene is etherified benzyl alcohol 70g, and 120 DEG C 2 hours in 5L autoclave are added in stannous octoate 0.2g, lactide 3000g After be warming up to 180 DEG C the reaction was continued 5 hours and to obtain off-white powder 3020g, be straight chain branched polylactide, yield 98.3%.
The straight chain branched polylactide is five branched polylactides, is detected through GPC:
Mn:19730, Mw/Mn=1.52, Mp:142 DEG C, crystallinity: 26.3%.
4) preparation of Water soluble diversion agent
By 89 parts of five branched polylactide, 5 parts of polytrimethylene carbonate PTMC, 5 parts of nano-corundum, antioxidant CA 0.3 Part, 0.7 part of silicone oil is put into mixer, mixing 8 minutes at 110 DEG C.Then double screw extruder is added in the good masterbatch of mixing Middle extruding pelletization, extrusion temperature are 100 DEG C of an area, 2nd area~110 DEG C of 4th area, 5th area~115 DEG C of tenth area, 11 area's temperature 110 ℃.Tie rod is squeezed out after extruder squeezes out, water cooling air-dries, and is granulated, obtains uniformly mixed plastic pellet, turns to be water-soluble To agent.
In order to examine a kind of actual performance of water-soluble diversion agent of the present invention, it is also necessary to be put into granular water-soluble diversion agent Diameter is in 8cm cylindrical shape punching block, and punching block has water filling port and water outlet up and down, carries out soluble test and bearing capacity test:
Rock core is put into punching block first, injects water, sealing frock is warming up to test temperature, is gradually forced into water outlet Outflow water records water flow;
Then water-soluble diversion agent obtained by embodiment being put into punching block on rock core again, pavement thickness 2cm, water is injected in compacting, Sealing frock, is warming up to test temperature, is gradually forced into water outlet outflow water, records water outlet after breakthrough pressure, and breakthrough Water flow;Temporarily stifled rate is calculated by formula (1).
(water flow after rock core water flow-breakthrough)/rock core water flow × 100%=temporarily blocks up rate (1)
In the case where keeping pressure and constant solution temperature, when temporary stifled rate is reduced to 0, show that diversion agent is completely molten Solution, record are completely dissolved the time.
The water-soluble diversion agent pressure of table 1, dissolution statistical form
The present invention is described by way of example above, but the present invention is not limited to above-mentioned specific embodiment, all to be based on Any changes or modifications that the present invention is done are fallen within the scope of the claimed invention.

Claims (5)

1. a kind of water-soluble diversion agent, which is characterized in that be prepared by following parts by weight of component:
Wherein, the straight chain branched polylactide is five branched polylactides;
The straight chain branched polylactide is polymerized by straight chain poly phosphazene and polylactide;
The straight chain poly phosphazene is the pentachloro- phosphine nitrile of the molecular weight that is polymerized by dichloro phosphine nitrile in 200-5000;
The straight chain poly phosphazene and the reaction equation of polylactide polymerization reaction are
2. water-soluble diversion agent as described in claim 1, which is characterized in that the straight chain branched polylactide is by following methods system It is standby to form:
Step (1): after hydroxy benzaldehyde in a kettle stirring and dissolving, catalyst reaction is added;Then pentachloro- phosphine nitrile is molten Solution, is slowly added dropwise in reaction kettle, is stirred to react;Finally reaction solution is filtered, merging filtrate, removes solvent, recrystallize to obtain phosphine Nitrile five is etherified benzaldehyde;
Step (2): reducing agent is dissolved to obtain reducing agent solution;The reduction is added dropwise to after phosphine nitrile five is etherified dissolution of benzaldehyde In agent solution, terminator is added after reaction, solvent is removed after fully reacting, extracts, stirring dries, filters and is spin-dried for filtering Liquid obtains phosphine nitrile five and is etherified benzyl alcohol;
Step (3): phosphine nitrile five is etherified benzyl alcohol, initiator and lactide and is added in autoclave, straight chain branch is made in hybrid reaction Change polylactide;
All components content is parts by weight.
3. water-soluble diversion agent as claimed in claim 2, which is characterized in that the catalyst is triethylamine, triisopropylamine, carbon One or more of sour potassium and sodium hydride;And/or the solvent is one or more of anhydrous THF or anhydrous propanone;Institute Stating reducing agent is sodium borohydride;And/or the terminator is the ammonium chloride solution of 5% concentration.
4. water-soluble diversion agent as described in claim 1, which is characterized in that the plasticizer is poly-hydroxy fatty acid, PEG, gathers One or more of trimethylene carbonate PTMC.
5. water-soluble diversion agent as described in claim 1, which is characterized in that the nanoreinforcement material is nanometer calcium carbonate, receives One or more of off-white carbon black, nanoscale talcum powder;And/or the antioxidant be antioxidant 1010, antioxidant 1076, One or more of antioxidant 164, antioxidant 264, antioxidant CA;And/or the lubricant is that stearic acid, stearic acid are sweet One or more of grease, paraffin, OPE wax, silicone oil.
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