CN103539893A - Preparation technology of water phase transmission drag reducer for slickwater fracturing - Google Patents
Preparation technology of water phase transmission drag reducer for slickwater fracturing Download PDFInfo
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Abstract
The invention discloses a preparation technology of a water phase transmission drag reducer for slickwater fracturing, and belongs to the field of oil field chemical water phase drag reduction technology. The preparation technology comprises following steps: an acrylamide monomer aqueous solution with a mass concentration of 18.5 to 25.5% is prepared; tert-butylacrylamide is added, wherein the content of tert-Butylacrylamide is 0.2 to 2.0wt% of that of the acrylamide monomer aqueous solution; sodium carbonate is added, wherein the content of sodium carbonate is 2.5 to 8.0wt% of that of the acrylamide monomer aqueous solution; a chelating agent, a chain transfer agent, a chain extender and a water soluble azo-compound are added; the mixture is subjected to polymerization and hydrolysis so as to obtain gel blocks; the gel blocks are processed so as to obtain polyacrylamide powder; and the polyacrylamide powder is mixed with sodium chloride particles so as to obtain the water phase transmission drag reducer. An optimized application concentration of the water phase transmission drag reducer ranges from 250 to 500ppm; compatibility with common bactericides, antiswelling agents and discharge aiding agents is excellent; solution formed by the water phase transmission drag reducer is stable; drag reduction efficiency is high and lasts long; influence of water mineralization degree on preparation of slickwater is less; and the water phase transmission drag reducer is suitable for water with more than 10% calcium chloride.
Description
Technical field
Slippery water water blanket transmits a preparation technology for flow improver mutually, belongs to oilfield chemistry water drag reduction technology field.
Background technology
Slickwater(slippery water) fracturing liquid is the main fracturing liquid of unconventional shale oil gas pressing crack construction, it is comprised of flow improver and other additive, and its key component is flow improver, mostly dependence on import, expensive, seriously hindered the exploitation of China's oil field shale gas resource.Therefore the slippery water pressure break friction reducer of, developing a kind of applicable oil field shale oil gas reservoir has important practice significance and economic benefit.
High polymer polyacrylamide can be used as water flow improver, in Halliburton slippery water, main component is anionic polyacrylamide (WO 2011/004141 A1, Improving Friction Reducer Performance in Water Containing Multivalent Ions), its commodity have FR series as FR-56, FR-48 etc., the aqueous solution for 15%-60% polymkeric substance and a small amount of sequestrant, by sequestrant, improve the Magnesium of Nai Gai divalent-metal ion ability, thereby improve drag-reduction effect and performance, but Halliburton oneself introduces, these FR series product are still used in clear water and less salt has drag-reduction effect, working concentration is 330ppm ~ 500ppm, polymkeric substance adopts Co-polypropylene acid amides, as acrylamide and acrylic copolymer, but there is no clear and definite monomer synthesis technique.By our research, monomer synthesis technique has remarkable effect to resistance reducing performance, patent WO 2011/004141 A1 method can not obtain the particularly flow improver of the Magnesium of Nai Gai divalent-metal ion ability of premium properties, its drag reducing efficiency is also 50% ~ 60%, even slippery water is when calcium chloride 1% is above, drag reducing efficiency is dropped rapidly to below 45%, and drag reducing efficiency loses gradually in time, has a strong impact on slippery water drag-reduction effect; Naco company (Comparing Friction Reducers ' Performance in Produced Water from Tight Gas Shales. JPT Nov. 2009) has comprised the comparison of Halliburton product resistance reducing performance by various flow improvers are on the market wherein actual, preferably the drag reducing efficiency of flow improver is 68%, its circular track test shows, its drag reduction onset time seriously lags behind, 2min could play drag-reduction effect, basic consistent with Halliburton patent report.So offshore company's flow improver that we rely at present, drag reducing efficiency is not high, do not surpass 70%, hydration onset speed is slow, the Magnesium of Nai Gai divalent-metal ion is indifferent, use for some time drag reducing efficiency to decline rapidly, even lost efficacy, show that high-salinity water quality can not be for preparing slippery water, there is huge challenge (Shawn M. Rimassa in the oil field water of slippery water, et al, Optimizing Fracturing Fluid from Flowback Water. SPE 125336, the 2009 SPE Tight Gas Completions Conference, San Antonio, Taxes, USA, 15-17 June 2009).
In oil and gas exploration and exploitation, slippery water fracturing liquid is widely used in the reservoir reconstruction of oil well and gasser, to reach the object of increase yields of oil and gas.In slippery water forms, water is undoubtedly the large consumption component of this technology, for environment and resource, consider, oil field produced water is the water resources of easily taking, therefore must a kind of Magnesium of Nai Gai divalent-metal ion ability of development strong use when long, the flow improver that drag-reduction effect decline is very little, meets slippery water fracturing technique needs.
Summary of the invention
The technical problem to be solved in the present invention is: overcome the deficiencies in the prior art, provide a kind of slippery water water blanket to transmit mutually the preparation technology of flow improver, the flow improver hydration onset speed that adopts this technique to prepare is fast, the Magnesium of resistance to calcium divalent-metal ion ability is strong.
The technical solution adopted for the present invention to solve the technical problems is: this slippery water water blanket transmits the preparation technology of flow improver mutually, it is characterized in that, concrete technology step is:
1, acrylamide is synthetic: vinyl cyanide and water are mixed according to volume ratio 1:6.5 ~ 7.5, then add Lei Nitong, carry out hydration reaction generate the acrylamide solution that mass concentration is 15.5% ~ 20.5% at 78 ~ 140 ℃;
2, acrylamide is concentrated: the acrylamide solution that is 15.5% ~ 20.5% by mass concentration is by the concentrated acrylamide monomer aqueous solution that obtains mass concentration 35% ~ 45%, and in the acrylamide monomer aqueous solution after concentrating, content of copper ion is controlled at below 5 ppm;
3, preparation monomer: it is 18.5 ~ 25.5% that the acrylamide monomer aqueous solution of mass concentration 35% ~ 45% is diluted with water to mass concentration, and add the N-tert-butyl acrylamide that accounts for acrylamide monomer aqueous solution weight 0.2 ~ 2.0% to prepare mixed solution, mixed solution is cooled to 7 ~ 10 ℃, stirs;
4, preparation reaction solution: add sodium carbonate or sodium carbonate solution to form reaction solution in the mixed solution of step 3, wherein the clean quality of sodium carbonate accounts for 2.5 ~ 8.0% of reaction solution quality, then accounts for reaction solution quality 20 ~ 100ppm sequestrant, 10 ~ 100ppm chain-transfer agent, 30 ~ 300ppm chain propagation agent and 50 ~ 250ppm water-soluble azo compounds to adding in reaction solution;
5, polymerization, hydrolysis: in reaction unit, lead to nitrogen deoxygenation and control reacting liquid temperature at 5 ~ 15 ℃, then add and account for the reductive agent of reaction solution quality 10 ~ 120ppm and the oxygenant of 10 ~ 120ppm, 10 ~ 15 ℃ of polymerizations 1 ~ 4 hour, then be warming up to 75 ~ 85 ℃ of hydrolysis 3 ~ 6 hours, after hydrolysis, obtain blob of viscose;
6, powder process: blob of viscose cutting, thin granulation drying treatment are obtained to polyacrylamide particle, then polyacrylamide particle is crushed and screened and obtains polyacrylamide powder; Polyacrylamide powder and sodium chloride particle are fully mixed and obtain flow improver, and wherein polyacrylamide accounts for 25 ~ 75% of flow improver weight.
Facts have proved, adopt the above-mentioned synthetic acrylamide monomer drag reducing efficiency of chemical method of the present invention to be greatly better than microbial method.The present invention optimizes the process that vinyl cyanide is prepared acrylamide of improving, specific hydration than and the condition of content of copper ion under make to react and met or exceeded the purity that microbial method is prepared acrylamide, compare and kept the advantage of high efficiency and the low investment of production of chemical preparation with microbial method.And in practice, the present invention states chemical method synthesis of acrylamide monomer drag reducing efficiency and is greatly better than microbial method.
Vinyl cyanide in described step 1 need carry out distilation at 78 ~ 95 ℃ before mixing, and it is standby that gas phase obtains fine propylene nitrile through condensation; Water in step 1 is preheated to 80 ℃ before mixing; Simmer down to flash distillation concentrate in described step 2.In order to remove moisture in vinyl cyanide, stopper and impurity, improve its purity, the vinyl cyanide in described step 1 need carry out distilation at 78 ~ 95 ℃ before mixing, and it is standby that gas phase obtains fine propylene nitrile through condensation; Water in described step 1 is preheated to 80 ℃ before mixing.
Simmer down to flash distillation concentrate in described step 2.The method that adopts flash distillation concentrate, is controlled at below 5 ppm content of copper ion in the acrylamide monomer aqueous solution.Under acrylamide monomer synthesis technique of the present invention, carry out when flash distillation concentrate obtains 35% ~ 45% the acrylamide monomer aqueous solution guaranteeing that content of copper ion is lower than 5 ppm.
Before adding, sodium carbonate in step 4 can be formulated as aqueous sodium carbonate, this step is in order to accelerate the dissolving of sodium carbonate in the acrylamide monomer aqueous solution, prevent precipitation, therefore at its concrete compound concentration, without sternly needing, strictly limit, reach sodium carbonate is dissolved, such as being the saturated solution of sodium carbonate; This can be chosen in the molten nonsurfactant that adds of aqueous sodium carbonate, and the consumption of nonsurfactant is no more than mixed solution and the aqueous sodium carbonate gross weight of 500ppm; Nonsurfactant is preferably Si Ban-40.In sodium carbonate described in step 4 or its solution, be evenly mixed with Si Ban-40 of 20 ~ 500ppm.
Preferably, the sequestrant in described step 4 is disodium ethylene diamine tetraacetate, and chain-transfer agent is sodium acetate, and chain propagation agent is Tetramethyl Ethylene Diamine, and water-soluble azo compounds is azo-bis-isobutyrate hydrochloride.The choice for use of disodium ethylene diamine tetraacetate, sodium acetate, Tetramethyl Ethylene Diamine and azo-bis-isobutyrate hydrochloride can make the polymerization degree of the poly-propionic acid amide that makes reach best drag-reduction effect and high-temperature resistant result.
Preferably, the reductive agent in described step 5 is sodium bisulfite, and oxygenant is Potassium Persulphate.
Logical nitrogen oxygen removal process described in step 5 was led to nitrogen 30min ~ 45min before adding reductive agent and oxygenant, added reductive agent and oxygenant to lead to afterwards nitrogen 5 ~ 15min again; Logical nitrogen deoxygenation is to making oxygen content < 200ppb in system.
In described step 6, the particle diameter of polyacrylamide particle is 3 ~ 5mm, and drying mode is for first dry at 85 ~ 110 ℃ with revolution percolation machine, then dry at 95 ℃ ~ 140 ℃ with vibration vulcanization bed; The particle diameter of polyacrylamide powder is 40 ~ 200 orders.
The working concentration scope of described flow improver in slippery water is 250ppm ~ 500ppm.Cross at most and can waste, not too large lifting of drag-reduction effect, was used and did not reach at least due result of use.The application method of the flow improver that above-mentioned preparation technology obtains, is about to above-mentioned flow improver and joins in slippery water and use as fracturing liquid.
The present invention improves the preparation technology of flow improver, main by the collocation of sequestrant used, chain-transfer agent, chain propagation agent and water-soluble azo compounds, make polymerization, the susceptibility variation of the blob of viscose that obtains of hydrolysis to impurity, id reaction is active to be strengthened.To meet the compatibility problems with quick water, under the poor condition of poor slippery water water quality, keep resistance reducing performance.
Compared with prior art, the beneficial effect that the preparation technology that a kind of slippery water water blanket of the present invention transmits flow improver mutually has is: the present invention mainly solves the compatibility problems of flow improver and quick water, prepared flow improver is by the performance evaluation of slippery water pressure break flow improver, with sterilant common in slippery water, expansion-resisting agent, cleanup additive compatibleness be good, it is solution-stabilized to form, drag reducing efficiency is high and long-acting, it is little that slippery water preparation is affected by water-mineralizing degree, can be suitable for calcium chloride content in 10% above water quality; The Molecular Weight for Polyacrylamide of flow improver is 1,400 ten thousand ~ 2,200 ten thousand, and degree of hydrolysis is 16.5% ~ 35.0%; Concrete effect is as follows:
1,, as flow improver, molten speed is fast, 30sec can be in slippery water rapidly hydration dissolve, 200ppm working concentration drag reducing efficiency reaches more than 70%, even up to 80%, good with the additive compatibleness such as component sterilant, expansion-resisting agent and cleanup additive in slippery water.
2, in containing 10% calcium chloride water, drag reducing efficiency is more than 68%, and after the long-term circular track test of 20min., drag reducing efficiency is still more than 60%.
Accompanying drawing explanation
Fig. 1 is that embodiment 1 flow improver working concentration is 490ppm drag reducing efficiency graphic representation over time.
Fig. 2 be embodiment 1 flow improver at 90 ℃ of drag reducing efficiencies with flow improver concentration curve.
Fig. 3 is that embodiment 2 flow improver working concentrations are 350ppm drag reducing efficiency graphic representation over time.
Fig. 4 is that embodiment 3 flow improver working concentrations are 420ppm drag reducing efficiency graphic representation over time.
Embodiment
The preparation technology of a kind of slippery water water blanket of the present invention being transmitted to flow improver mutually below by specific embodiment is described further, and wherein embodiment 1 is most preferred embodiment.Reagent Si Ban-40 used are the common product of common commercially available chemical pure level, there is no particular requirement.
Embodiment 1
One, the preparation process of flow improver is as follows:
1, will refine vinyl cyanide and pure water by volume 1:7 mix, add Lei Nitong, be heated to 110 ~ 120 ℃, hydration reaction generates the acrylamide solution that mass concentration is 16%, by flash distillation concentrate, obtain 40% the acrylamide monomer aqueous solution, content of copper ion is below 5 ppm, as synthesizing one of raw material monomer of flow improver;
2, the aforesaid propylene amide monomer aqueous solution is diluted with water to 22.0%, adds the N-tert-butyl acrylamide that accounts for acrylamide monomer aqueous solution weight 1.5%, mixed solution is refrigerated to 7 ℃ of temperature, in material-compound tank, is uniformly mixed;
3, the sodium carbonate of mixed solution weight 4.7% will be accounted for, first add water dissolution wiring solution-forming, then under constantly stirring, be added in above-mentioned mixed solution, after stirring, add successively the EDETATE SODIUM (being disodium ethylene diamine tetraacetate), the sodium acetate of 20ppm, the water-soluble azo compounds azo-bis-isobutyrate hydrochloride of the Tetramethyl Ethylene Diamine of 300ppm, 100ppm that account for reaction system 80ppm,, obtaining transparent or translucent solution, solution temperature is controlled at 13 ~ 15 ℃;
4, above-mentioned solution is pumped into polymeric kettle, temperature is controlled at 13 ~ 15 ℃, be filled with High Purity Nitrogen 30min, then to polymeric kettle, add the reductive agent sodium bisulfite of 38ppm, the oxygenant Potassium Persulphate of 38ppm, continues logical nitrogen 15min, polymerization temperature is controlled at 13 ~ 15 ℃, reaction times is 1 ~ 4 hour, after polymerization, in 85 ℃ of hydrolysis 4 hours, after hydrolysis, blob of viscose is extruded with pressurized air;
5, by the cutting of above-mentioned blob of viscose, thin granulation, obtain the polyacrylamide gel particles of 3 ~ 5mm, be delivered to revolution percolation machine and be dried, temperature is controlled at 85 ~ 110 ℃, and then enters vibration vulcanization bed and be dried, and temperature is controlled at 95 ℃ ~ 140 ℃;
6, by above-mentioned dried polyacrylamide particle through screening, then enter pulverizing mill abrasive dust, Vibration Screen separately wins 40 ~ 200 order powders, cooling;
7, above-mentioned powder is measured than mixing by 7:3 with sodium chloride particle, in Agravicmixer, fully mix, be flow improver, the molecular weight of the polyacrylamide of actual measurement flow improver is 1,820 ten thousand, degree of hydrolysis 29.8%, and polyacrylamide amine content is 72.2%.
Two, resistance reducing performance evaluation: good with slippery water compatibleness, at content, be (in slippery water, also to contain 1% Repone K) in 1% calcium chloride slippery water, Fig. 1 is shown in drag-reduction effect evaluation, and flow improver is onset immediately within half a minute, drag reducing efficiency is basic in 20min not to decline, and maintains more than 75%.And time and drag reducing efficiency graph of a relation that Halliburton patent WO 2011/004141 A1 shows, the maximum drag reducing efficiency that 2min reaches is 65%, calcium chloride content is only 0.15%, is significantly less than 1% in the present invention.
Fig. 2 is that the present embodiment flow improver drag reducing efficiency in the time of 90 ℃, with flow improver concentration curve, shows that the best working concentration of flow improver that the present invention produces is at 250 ~ 500ppm, i.e. flow improver prepared by the present invention is anticalcium not only, and heatproof.
Embodiment 2
One, the preparation process of flow improver is as follows:
1, will refine vinyl cyanide and water by volume 1:7 mix, add Lei Nitong, be heated to 110 ~ 130 ℃, hydration reaction generates the acrylamide solution that mass concentration is 15.5% ~ 20.5%, by flash distillation concentrate, obtain 38% the acrylamide monomer aqueous solution, content of copper ion is below 5 ppm, as synthesizing one of raw material monomer of flow improver;
2, the above-mentioned pure acrylamide monomer aqueous solution is diluted with water to 21.5%, adds the N-tert-butyl acrylamide that accounts for acrylamide monomer aqueous solution weight 1.0%, mixed solution is refrigerated to temperature below 8 ℃, in material-compound tank, is uniformly mixed;
3, the sodium carbonate of mixed solution weight 4.7% will be accounted for, first add water dissolution wiring solution-forming, and in solution, add Si Ban-40, its consumption is mixed solution and the aqueous sodium carbonate gross weight that the step (2) of 250ppm obtains, then sodium carbonate solution is added in above-mentioned mixed solution under constantly stirring, after stirring, add successively and account for reaction system 60ppmEDTA disodium, the sodium acetate of 40ppm, the Tetramethyl Ethylene Diamine of 80ppm, the water-soluble azo compounds azo-bis-isobutyrate hydrochloride of 125ppm, obtain transparent or translucent solution, solution temperature is controlled at below 15 ℃,
4, above-mentioned solution is pumped into polymeric kettle, temperature is controlled at 12 ~ 15 ℃, be filled with High Purity Nitrogen 30min, then to polymeric kettle, add the reductive agent sodium bisulfite of 60ppm, the oxygenant Potassium Persulphate of 60ppm, continues logical nitrogen 15min, polymerization temperature is controlled at 12 ~ 15 ℃, reaction times is 1-4 hour, after polymerization, in 85 ℃ of hydrolysis 6 hours, after hydrolysis, blob of viscose is extruded with pressurized air;
5, by the cutting of above-mentioned blob of viscose, thin granulation, obtain the polyacrylamide gel particles of 3 ~ 5mm, be delivered to revolution percolation machine and be dried, temperature is controlled at 85 ~ 110 ℃, and then enters vibration vulcanization bed and be dried, and temperature is controlled at 95 ℃ ~ 140 ℃;
6, by above-mentioned dried polyacrylamide particle through screening, then enter pulverizing mill abrasive dust, Vibration Screen separately wins 40 ~ 200 order powders, cooling;
7, above-mentioned powder is measured than mixing by 3:7 with sodium chloride particle, in Agravicmixer, fully mix, be flow improver, in actual measurement flow improver, the molecular weight of polyacrylamide is 1,980 ten thousand, degree of hydrolysis 31.8%, and polyacrylamide amine content is 72.2%.
Resistance reducing performance is evaluated: good with slippery water compatibleness, at content, be (in slippery water, also to contain 1% Repone K) in 10% calcium chloride slippery water, Fig. 3 is shown in drag-reduction effect evaluation, drag reducing efficiency is more than 70%, and drag reducing efficiency temporal evolution is steady, after 20min, drag reducing efficiency, still up to 68.8%, shows the high anticalcium of product, and drag reduction is long-acting.
Embodiment 3
One, the preparation process of flow improver is as follows:
1, will refine vinyl cyanide and water by volume 1:7 mix, add Lei Nitong, be heated to 95 ~ 140 ℃, hydration reaction generates the acrylamide solution that mass concentration is 15.5% ~ 20.5%, by flash distillation concentrate, obtain 42% the acrylamide monomer aqueous solution, content of copper ion is below 5 ppm, as synthesizing one of raw material monomer of flow improver;
2, the above-mentioned pure acrylamide monomer aqueous solution is diluted with water to 22.0%,, add the N-tert-butyl acrylamide that accounts for acrylamide monomer aqueous solution weight 1.2%, mixed solution is refrigerated to temperature below 8 ℃, in material-compound tank, is uniformly mixed;
3, the sodium carbonate of mixed solution weight 3.6% will be accounted for, first add water dissolution wiring solution-forming, under constantly stirring, be added in above-mentioned mixed solution, after stirring, add successively and account for the EDETATE SODIUM of reaction system 80ppm, the water-soluble azo compounds azo-bis-isobutyrate hydrochloride of the Tetramethyl Ethylene Diamine of the sodium acetate of 20ppm, 150ppm, 180ppm, obtain transparent or translucent solution, solution temperature is controlled at below 15 ℃;
4, above-mentioned solution is pumped into polymeric kettle, temperature is controlled at 11 ~ 13 ℃, be filled with High Purity Nitrogen 30min, then to polymeric kettle, add the reductive agent sodium bisulfite of 80ppm, the oxygenant Potassium Persulphate of 80ppm, continues logical nitrogen 15min, polymerization temperature is controlled at 11 ~ 13 ℃, reaction times is 1 ~ 4 hour, after polymerization, in 85 ℃ of hydrolysis 5 hours, after hydrolysis, blob of viscose is extruded with pressurized air;
5, by the cutting of above-mentioned blob of viscose, thin granulation, obtain the polyacrylamide gel particles of 3 ~ 5mm, be delivered to revolution percolation machine and be dried, temperature is controlled at 85 ~ 110 ℃, and then enters vibration vulcanization bed and be dried, and temperature is controlled at 95 ℃ ~ 140 ℃;
6, by above-mentioned dried polyacrylamide particle through screening, then enter pulverizing mill abrasive dust, Vibration Screen separately wins 40 ~ 200 order powders, cooling;
7, above-mentioned powder is measured than mixing by 7:3 with sodium chloride particle, in Agravicmixer, fully mix, be flow improver, the molecular weight of actual measurement flow improver polyacrylamide is 2,050 ten thousand, degree of hydrolysis 21.3%, and polyacrylamide amine content is 70.6%.
Two, resistance reducing performance evaluation: be (also to contain 1% Repone K in slippery water) in 5% calcium chloride slippery water at content, Fig. 4 is shown in drag-reduction effect evaluation, drag reducing efficiency is more than 70%, and drag reducing efficiency temporal evolution is steady, after 20min, drag reducing efficiency is still up to 78.5%, show the high anticalcium of product, drag reduction is long-acting.
Embodiment 4
One, the preparation process of flow improver is as follows:
1, will refine vinyl cyanide and pure water by volume 1:7.5 mix, add Lei Nitong, be heated to 78 ℃, hydration reaction generates the acrylamide solution that mass concentration is 15.5%, by flash distillation concentrate, obtain 35% the acrylamide monomer aqueous solution, content of copper ion is below 5 ppm, as synthesizing one of raw material monomer of flow improver;
2, the aforesaid propylene amide monomer aqueous solution is diluted with water to 18.5%, adds the N-tert-butyl acrylamide that accounts for acrylamide monomer aqueous solution weight 0.2%, mixed solution is refrigerated to 6 ~ 8 ℃ of temperature, in material-compound tank, is uniformly mixed;
3, the sodium carbonate that accounts for mixed solution weight 2.5% is added in above-mentioned mixing solutions under constantly stirring, after stirring, add successively the EDETATE SODIUM (being disodium ethylene diamine tetraacetate), the sodium acetate of 10ppm, the water-soluble azo compounds azo-bis-isobutyrate hydrochloride of the Tetramethyl Ethylene Diamine of 30ppm, 50ppm that account for reaction system 20ppm, obtain transparent or translucent solution, solution temperature is controlled at 10-14 ℃;
4, above-mentioned solution is pumped into polymeric kettle, temperature is controlled at 10 ~ 12 ℃, be filled with High Purity Nitrogen 30min, then to polymeric kettle, add the reductive agent sodium bisulfite of 10ppm, the oxygenant Potassium Persulphate of 10ppm, continues logical nitrogen 5min to oxygen content < 200ppb in system, polymerization temperature is controlled at 10 ~ 12 ℃, reaction times is 1 hour, after polymerization, in 85 ℃ of hydrolysis 3 hours, after hydrolysis, blob of viscose is extruded with pressurized air;
5, by the cutting of above-mentioned blob of viscose, thin granulation, obtain the polyacrylamide gel particles of 3 ~ 5mm, be delivered to revolution percolation machine and be dried, temperature is controlled at 85 ~ 110 ℃, and then enters vibration vulcanization bed and be dried, and temperature is controlled at 95 ℃ ~ 140 ℃;
6, by above-mentioned dried polyacrylamide particle through screening, then enter pulverizing mill abrasive dust, Vibration Screen separately wins 40 ~ 200 order powders, cooling;
7, above-mentioned powder is measured than mixing by 3:7 with sodium chloride particle, in Agravicmixer, fully mix, be flow improver, the molecular weight of actual measurement flow improver is 1,560 ten thousand, degree of hydrolysis 16.5%, and polyacrylamide amine content is 30.6%.
Two, resistance reducing performance evaluation: good with slippery water compatibleness, at content, be (in slippery water, also to contain 1% Repone K) in 1% calcium chloride slippery water, can access drag-reduction effect similarly to Example 1.
One, the preparation process of flow improver is as follows:
1, will refine vinyl cyanide and pure water by volume 1:6.5 mix, add Lei Nitong, be heated to 140 ℃, hydration reaction generates the acrylamide solution that mass concentration is 20.5%, by flash distillation concentrate, obtain 45% the acrylamide monomer aqueous solution, content of copper ion is below 5 ppm, as synthesizing one of raw material monomer of flow improver;
2, the aforesaid propylene amide monomer aqueous solution is diluted with water to 25.5%, adds the N-tert-butyl acrylamide that accounts for acrylamide monomer aqueous solution weight 2.0%, mixed solution is refrigerated to 6 ~ 8 ℃ of temperature, in material-compound tank, is uniformly mixed;
3, the sodium carbonate of mixed solution weight 8.0% will be accounted for, first add water dissolution wiring solution-forming, and in solution, add Si Ban-40, its consumption is mixed solution and the aqueous sodium carbonate gross weight that the step (2) of 500ppm obtains, then sodium carbonate solution is added in above-mentioned mixed solution under constantly stirring, after stirring, add successively the EDETATE SODIUM (being disodium ethylene diamine tetraacetate) that accounts for reaction system 100ppm, the sodium acetate of 100ppm, the Tetramethyl Ethylene Diamine of 100ppm, the water-soluble azo compounds azo-bis-isobutyrate hydrochloride of 250ppm, , obtain transparent or translucent solution, solution temperature is controlled at 6 ~ 8 ℃,
4, above-mentioned solution is pumped into polymeric kettle, temperature is controlled at 8 ~ 10 ℃, be filled with High Purity Nitrogen 45min, then to polymeric kettle, add the reductive agent sodium bisulfite of 120ppm, the oxygenant Potassium Persulphate of 120ppm, continues logical nitrogen 15min to oxygen content < 200ppb in system, polymerization temperature is controlled at 8 ~ 10 ℃, reaction times is 4 hours, after polymerization, in 75 ℃ of hydrolysis 6 hours, after hydrolysis, blob of viscose is extruded with pressurized air;
5, by the cutting of above-mentioned blob of viscose, thin granulation, obtain the polyacrylamide gel particles of 3 ~ 5mm, be delivered to revolution percolation machine and be dried, temperature is controlled at 85 ~ 110 ℃, and then enters vibration vulcanization bed and be dried, and temperature is controlled at 95 ℃ ~ 140 ℃;
6, by above-mentioned dried polyacrylamide particle through screening, then enter pulverizing mill abrasive dust, Vibration Screen separately wins 40 ~ 200 order powders, cooling;
7, above-mentioned powder is measured than mixing by 4:6 with sodium chloride particle, in Agravicmixer, fully mix, be flow improver, the molecular weight of actual measurement flow improver polyacrylamide is 2,200 ten thousand, degree of hydrolysis 35%, and polyacrylamide amine content is 58.8%.
Two, resistance reducing performance evaluation: good with slippery water compatibleness, at content, be (in slippery water, also to contain 1% Repone K) in 10% calcium chloride slippery water, can access drag-reduction effect similarly to Example 2.
Embodiment 6
One, the preparation process of flow improver is as follows:
1, will refine vinyl cyanide and pure water by volume 1:7 mix, add Lei Nitong, be heated to 140 ℃, hydration reaction generates the acrylamide solution that mass concentration is 18%, by flash distillation concentrate, obtain 45% the acrylamide monomer aqueous solution, content of copper ion is below 5 ppm, as synthesizing one of raw material monomer of flow improver;
2, the aforesaid propylene amide monomer aqueous solution is diluted with water to 22%, adds the N-tert-butyl acrylamide that accounts for acrylamide monomer aqueous solution weight 1.0%, mixed solution is refrigerated to 5 ~ 8 ℃ of temperature, in material-compound tank, is uniformly mixed;
3, the sodium carbonate of mixed solution weight 5.5% will be accounted for, first add water dissolution wiring solution-forming, and in solution, add Si Ban-40, its consumption is mixed solution and the aqueous sodium carbonate gross weight that the step (2) of 20ppm obtains, then sodium carbonate solution is added in above-mentioned mixed solution under constantly stirring, after stirring, add successively the EDETATE SODIUM (being disodium ethylene diamine tetraacetate) that accounts for reaction system 60ppm, the sodium acetate of 50ppm, the Tetramethyl Ethylene Diamine of 180ppm, the water-soluble azo compounds azo-bis-isobutyrate hydrochloride of 150ppm, , obtain transparent or translucent solution, solution temperature is controlled at 5 ~ 8 ℃,
4, above-mentioned solution is pumped into polymeric kettle, temperature is controlled at 5 ~ 9 ℃, be filled with High Purity Nitrogen 40min, then to polymeric kettle, add the reductive agent sodium bisulfite of 60ppm, the oxygenant Potassium Persulphate of 60ppm, continues logical nitrogen 10min to oxygen content < 200ppb in system, polymerization temperature is controlled at 5 ~ 9 ℃, reaction times is 2.5 hours, after polymerization, in 85 ℃ of hydrolysis 4.5 hours, after hydrolysis, blob of viscose is extruded with pressurized air;
5, by the cutting of above-mentioned blob of viscose, thin granulation, obtain the polyacrylamide gel particles of 3 ~ 5mm, be delivered to revolution percolation machine and be dried, temperature is controlled at 85 ~ 110 ℃, and then enters vibration vulcanization bed and be dried, and temperature is controlled at 95 ℃ ~ 140 ℃;
6, by above-mentioned dried polyacrylamide particle through screening, then enter pulverizing mill abrasive dust, Vibration Screen separately wins 40 ~ 200 order powders, cooling;
7, above-mentioned powder is measured than mixing by 5:5 with sodium chloride particle, in Agravicmixer, fully mix, be flow improver, the molecular weight of actual measurement flow improver polyacrylamide is 1,940 ten thousand, degree of hydrolysis 33.4%, and polyacrylamide amine content is 50.2%.
Two, resistance reducing performance evaluation: good with slippery water compatibleness, at content, be (in slippery water, also to contain 1% Repone K) in 5% calcium chloride slippery water, can access drag-reduction effect similarly to Example 3.
Comparative example 1
One, the preparation process of flow improver is as follows:
1, will refine vinyl cyanide and pure water by volume 1:7 mix, add Lei Nitong, be heated to 140 ℃, hydration reaction generates the acrylamide solution that mass concentration is 18%, by flash distillation concentrate, obtain 45% the acrylamide monomer aqueous solution, content of copper ion is below 5 ppm, as synthesizing one of raw material monomer of flow improver;
2, the aforesaid propylene amide monomer aqueous solution is diluted with water to 22%, adds the N-tert-butyl acrylamide that accounts for acrylamide monomer aqueous solution weight 1.0%, mixed solution is refrigerated to 5 ~ 8 ℃ of temperature, in material-compound tank, is uniformly mixed;
3, the sodium carbonate of mixed solution weight 5.5% will be accounted for, first add water dissolution wiring solution-forming, and in solution, add Si Ban-40, its consumption is mixed solution and the aqueous sodium carbonate gross weight that the step (2) of 20ppm obtains, then sodium carbonate solution is added in above-mentioned mixed solution under constantly stirring, after stirring, add successively the EDETATE SODIUM (being disodium ethylene diamine tetraacetate) that accounts for reaction system 10ppm, the sodium acetate of 5ppm, the Tetramethyl Ethylene Diamine of 500ppm, the water-soluble azo compounds azo-bis-isobutyrate hydrochloride of 300ppm, , obtain transparent or translucent solution, solution temperature is controlled at 5 ~ 8 ℃,
4, above-mentioned solution is pumped into polymeric kettle, temperature is controlled at 5 ~ 9 ℃, be filled with High Purity Nitrogen 40min, then to polymeric kettle, add the reductive agent sodium bisulfite of 60ppm, the oxygenant Potassium Persulphate of 60ppm, continues logical nitrogen 10min to oxygen content < 200ppb in system, polymerization temperature is controlled at 5 ~ 9 ℃, reaction times is 2.5 hours, after polymerization, in 85 ℃ of hydrolysis 4.5 hours, after hydrolysis, blob of viscose is extruded with pressurized air;
5, by the cutting of above-mentioned blob of viscose, thin granulation, obtain the polyacrylamide gel particles of 3 ~ 5mm, be delivered to revolution percolation machine and be dried, temperature is controlled at 85 ~ 110 ℃, and then enters vibration vulcanization bed and be dried, and temperature is controlled at 95 ℃ ~ 140 ℃;
6, by above-mentioned dried polyacrylamide particle through screening, then enter pulverizing mill abrasive dust, Vibration Screen separately wins 40 ~ 200 order powders, cooling;
7, above-mentioned powder is measured than mixing by 5:5 with sodium chloride particle, in Agravicmixer, fully mix, be flow improver, the molecular weight of actual measurement flow improver polyacrylamide is 1,940 ten thousand, degree of hydrolysis 33.4%, and polyacrylamide amine content is 50.2%.
Two, resistance reducing performance evaluation: general with slippery water compatibleness, at content, be (in slippery water, also to contain 1% Repone K) in 5% calcium chloride slippery water, drag-reduction effect is evaluated poor, drag reducing efficiency only has 50%, and drag reducing efficiency increases in time and reduces, after 50min, drag reducing efficiency only has 30%, show that anticalcium performance is undesirable, and the drag reduction time is shorter.
Comparative example 2
One, the preparation process of flow improver is as follows:
1, will refine vinyl cyanide and pure water by volume 1:7 mix, add Lei Nitong, be heated to 140 ℃, hydration reaction generates the acrylamide solution that mass concentration is 18%, by flash distillation concentrate, obtain 45% the acrylamide monomer aqueous solution, content of copper ion is below 5 ppm, as synthesizing one of raw material monomer of flow improver;
2, the aforesaid propylene amide monomer aqueous solution is diluted with water to 22%, adds the N-tert-butyl acrylamide that accounts for acrylamide monomer aqueous solution weight 1.0%, mixed solution is refrigerated to 10 ℃ of temperature, in material-compound tank, is uniformly mixed;
3, the sodium carbonate of mixed solution weight 5.5% will be accounted for, first add water dissolution wiring solution-forming, and in solution, add Si Ban-40, its consumption is mixed solution and the aqueous sodium carbonate gross weight that the step (2) of 20ppm obtains, then sodium carbonate solution is added in above-mentioned mixed solution under constantly stirring, after stirring, add successively the EDETATE SODIUM (being disodium ethylene diamine tetraacetate) that accounts for reaction system 60ppm, the sodium acetate of 50ppm, the Tetramethyl Ethylene Diamine of 180ppm, the water-soluble azo compounds azo-bis-isobutyrate hydrochloride of 150ppm, , obtain transparent or translucent solution, solution temperature is controlled at 5 ~ 8 ℃,
4, above-mentioned solution is pumped into polymeric kettle, temperature is controlled at 20 ℃, be filled with High Purity Nitrogen 40min, then to polymeric kettle, add the reductive agent sodium bisulfite of 60ppm, the oxygenant Potassium Persulphate of 60ppm, continues logical nitrogen 10min to oxygen content < 200ppb in system, polymerization temperature is controlled at 20 ℃, reaction times is 2.5 hours, after polymerization, in 60 ℃ of hydrolysis 4.5 hours, after hydrolysis, blob of viscose is extruded with pressurized air;
5, by the cutting of above-mentioned blob of viscose, thin granulation, obtain the polyacrylamide gel particles of 3 ~ 5mm, be delivered to revolution percolation machine and be dried, temperature is controlled at 85 ~ 110 ℃, and then enters vibration vulcanization bed and be dried, and temperature is controlled at 95 ℃ ~ 140 ℃;
6, by above-mentioned dried polyacrylamide particle through screening, then enter pulverizing mill abrasive dust, Vibration Screen separately wins 40 ~ 200 order powders, cooling;
7, above-mentioned powder is measured than mixing by 5:5 with sodium chloride particle, in Agravicmixer, fully mix, be flow improver, the molecular weight of actual measurement flow improver polyacrylamide is 1,940 ten thousand, degree of hydrolysis 33.4%, and polyacrylamide amine content is 50.2%.
Two, resistance reducing performance evaluation: general with slippery water compatibleness, at content, be (in slippery water, also to contain 1% Repone K) in 5% calcium chloride slippery water, drag-reduction effect is evaluated poor, drag reducing efficiency only has 55%, and drag reducing efficiency increases in time and reduces, after 20min, drag reducing efficiency only has 32%, show that anticalcium performance is undesirable, and the drag reduction time is shorter.
Comparative example 3
One, the preparation process of flow improver is as follows:
1, the acrylamide monomer that adopts traditional microbial method to produce, thin up is 22% the acrylamide monomer aqueous solution, add the N-tert-butyl acrylamide that accounts for acrylamide monomer aqueous solution weight 1.0%, mixed solution is refrigerated to 10 ℃ of temperature, in material-compound tank, is uniformly mixed;
2, the sodium carbonate of mixed solution weight 5.5% will be accounted for, first add water dissolution wiring solution-forming, and in solution, add Si Ban-40, its consumption is mixed solution and the aqueous sodium carbonate gross weight that the step 1 of 20ppm obtains, then sodium carbonate solution is added in above-mentioned mixed solution under constantly stirring, after stirring, add successively the EDETATE SODIUM (being disodium ethylene diamine tetraacetate) that accounts for reaction system 60ppm, the sodium acetate of 50ppm, the Tetramethyl Ethylene Diamine of 180ppm, the water-soluble azo compounds azo-bis-isobutyrate hydrochloride of 150ppm, , obtain transparent or translucent solution, solution temperature is controlled at 5 ~ 8 ℃,
3, above-mentioned solution is pumped into polymeric kettle, temperature is controlled at 20 ℃, be filled with High Purity Nitrogen 40min, then to polymeric kettle, add the reductive agent sodium bisulfite of 60ppm, the oxygenant Potassium Persulphate of 60ppm, continues logical nitrogen 10min to oxygen content < 200ppb in system, polymerization temperature is controlled at 20 ℃, reaction times is 2.5 hours, after polymerization, in 60 ℃ of hydrolysis 4.5 hours, after hydrolysis, blob of viscose is extruded with pressurized air;
4, by the cutting of above-mentioned blob of viscose, thin granulation, obtain the polyacrylamide gel particles of 3 ~ 5mm, be delivered to revolution percolation machine and be dried, temperature is controlled at 85 ~ 110 ℃, and then enters vibration vulcanization bed and be dried, and temperature is controlled at 95 ℃ ~ 140 ℃;
5, by above-mentioned dried polyacrylamide particle through screening, then enter pulverizing mill abrasive dust, Vibration Screen separately wins 40 ~ 200 order powders, cooling;
6, above-mentioned powder is measured than mixing by 5:5 with sodium chloride particle, in Agravicmixer, fully mix, be flow improver, the molecular weight of actual measurement flow improver polyacrylamide is 1,940 ten thousand, degree of hydrolysis 33.4%, and polyacrylamide amine content is 50.2%.
Two, resistance reducing performance evaluation: good with slippery water compatibleness, at content, be (in slippery water, also to contain 1% Repone K) in 5% calcium chloride slippery water, drag-reduction effect evaluation is general, drag reducing efficiency is 65%, and drag reducing efficiency increases in time and reduces, after 20min, drag reducing efficiency remains on 55 ~ 45%, show that anticalcium performance is still not ideal, and the drag reduction time is shorter.
Comparative example 4
One, the preparation process of flow improver is as follows:
1, will refine vinyl cyanide and pure water by volume 1:5 mix, add Lei Nitong, be heated to 140 ℃, hydration reaction generates the acrylamide solution that mass concentration is 21%, by flash distillation concentrate, obtain 45% the acrylamide monomer aqueous solution, detect content of copper ion at 5.5ppm;
2, the aforesaid propylene amide monomer aqueous solution is diluted with water to 22%, adds the N-tert-butyl acrylamide that accounts for acrylamide monomer aqueous solution weight 1.0%, mixed solution is refrigerated to 10 ℃ of temperature, in material-compound tank, is uniformly mixed;
3, the sodium carbonate of mixed solution weight 5.5% will be accounted for, first add water dissolution wiring solution-forming, and in solution, add Si Ban-40, its consumption is mixed solution and the aqueous sodium carbonate gross weight that the step (2) of 20ppm obtains, then sodium carbonate solution is added in above-mentioned mixed solution under constantly stirring, after stirring, add successively the EDETATE SODIUM (being disodium ethylene diamine tetraacetate) that accounts for reaction system 60ppm, the sodium acetate of 50ppm, the Tetramethyl Ethylene Diamine of 180ppm, the water-soluble azo compounds azo-bis-isobutyrate hydrochloride of 150ppm, , obtain transparent or translucent solution, solution temperature is controlled at 5 ~ 8 ℃,
4, above-mentioned solution is pumped into polymeric kettle, temperature is controlled at 20 ℃, be filled with High Purity Nitrogen 40min, then to polymeric kettle, add the reductive agent sodium bisulfite of 60ppm, the oxygenant Potassium Persulphate of 60ppm, continues logical nitrogen 10min to oxygen content < 200ppb in system, polymerization temperature is controlled at 20 ℃, reaction times is 2.5 hours, after polymerization, in 60 ℃ of hydrolysis 4.5 hours, after hydrolysis, blob of viscose is extruded with pressurized air;
5, by the cutting of above-mentioned blob of viscose, thin granulation, obtain the polyacrylamide gel particles of 3 ~ 5mm, be delivered to revolution percolation machine and be dried, temperature is controlled at 85 ~ 110 ℃, and then enters vibration vulcanization bed and be dried, and temperature is controlled at 95 ℃ ~ 140 ℃;
6, by above-mentioned dried polyacrylamide particle through screening, then enter pulverizing mill abrasive dust, Vibration Screen separately wins 40 ~ 200 order powders, cooling;
7, above-mentioned powder is measured than mixing by 5:5 with sodium chloride particle, in Agravicmixer, fully mix, be flow improver, the molecular weight of actual measurement flow improver polyacrylamide is 1,740 ten thousand, degree of hydrolysis 31.4%, and polyacrylamide amine content is 50.2%.
Two, resistance reducing performance evaluation: general with slippery water compatibleness, at content, be (in slippery water, also to contain 1% Repone K) in 5% calcium chloride slippery water, drag-reduction effect evaluation is general, drag reducing efficiency is 60%, and drag reducing efficiency increases in time and reduce, after 20min, drag reducing efficiency is 54%, shows that anticalcium performance is not ideal, and resistance reducing performance extends in time to some extent and to decline, practical function is not ideal enough.
Comparative example 5
One, the preparation process of flow improver is as follows:
1, will refine vinyl cyanide and pure water by volume 1:9 mix, add Lei Nitong, be heated to 140 ℃, hydration reaction generates the acrylamide solution that mass concentration is 8%, by flash distillation concentrate, obtain 40% the acrylamide monomer aqueous solution, detect content of copper ion below 5ppm;
2, the aforesaid propylene amide monomer aqueous solution is diluted with water to 22%, adds the N-tert-butyl acrylamide that accounts for acrylamide monomer aqueous solution weight 1.0%, mixed solution is refrigerated to 10 ℃ of temperature, in material-compound tank, is uniformly mixed;
3, the sodium carbonate of mixed solution weight 5.5% will be accounted for, first add water dissolution wiring solution-forming, and in solution, add Si Ban-40, its consumption is mixed solution and the aqueous sodium carbonate gross weight that the step (2) of 20ppm obtains, then sodium carbonate solution is added in above-mentioned mixed solution under constantly stirring, after stirring, add successively the EDETATE SODIUM (being disodium ethylene diamine tetraacetate) that accounts for reaction system 60ppm, the sodium acetate of 50ppm, the Tetramethyl Ethylene Diamine of 180ppm, the water-soluble azo compounds azo-bis-isobutyrate hydrochloride of 150ppm, , obtain transparent or translucent solution, solution temperature is controlled at 5 ~ 8 ℃,
4, above-mentioned solution is pumped into polymeric kettle, temperature is controlled at 20 ℃, be filled with High Purity Nitrogen 40min, then to polymeric kettle, add the reductive agent sodium bisulfite of 60ppm, the oxygenant Potassium Persulphate of 60ppm, continues logical nitrogen 10min to oxygen content < 200ppb in system, polymerization temperature is controlled at 20 ℃, reaction times is 2.5 hours, after polymerization, in 60 ℃ of hydrolysis 4.5 hours, after hydrolysis, blob of viscose is extruded with pressurized air;
5, by the cutting of above-mentioned blob of viscose, thin granulation, obtain the polyacrylamide gel particles of 3 ~ 5mm, be delivered to revolution percolation machine and be dried, temperature is controlled at 85 ~ 110 ℃, and then enters vibration vulcanization bed and be dried, and temperature is controlled at 95 ℃ ~ 140 ℃;
6, by above-mentioned dried polyacrylamide particle through screening, then enter pulverizing mill abrasive dust, Vibration Screen separately wins 40 ~ 200 order powders, cooling;
7, above-mentioned powder is measured than mixing by 5:5 with sodium chloride particle, in Agravicmixer, fully mix, be flow improver, the molecular weight of actual measurement flow improver polyacrylamide is 1,950 ten thousand, degree of hydrolysis 33.6%, and polyacrylamide amine content is 50%.
Two, resistance reducing performance evaluation: general with slippery water compatibleness, at content, be (in slippery water, also to contain 1% Repone K) in 5% calcium chloride slippery water, drag-reduction effect evaluation is general, drag reducing efficiency is 69%, and drag reducing efficiency increases in time and reduce, after 20min, drag reducing efficiency, 65%, shows that anticalcium performance is not ideal, and resistance reducing performance extends in time and have downtrending, practical function each embodiment declines to some extent.And when prepared by this embodiment acrylamide solution due to low hydration ratio, production efficiency also can decline greatly, and increases concentrate difficulty.
By above embodiment and comparative example, can be found out, under processing condition of the present invention, coordinate each additive of sequestrant, chain-transfer agent, chain propagation agent and water-soluble azo compounds of amount of the present invention just can make the adaptive faculty grow of flow improver to water quality, the in the situation that of poor water quality, keep the drag-reduction effect of efficient drag reducing efficiency and long period.If comparative example 1 and embodiment contrast can find that the add-on of each additive changes, still undesirable with the flow improver performance making under processing condition, effect is poor.Comparative example 2 and embodiment contrast can find that at preparation process condition, controlling improper is to have a strong impact on flow improver performance, but effect is little compared with the add-on impact of additive.The acrylamide monomer that uses traditional microbial method to prepare in comparative example 3, in the situation that polyacrylamide and flow improver preparation process are identical with conditionally complete, drag-reduction effect evaluation slightly promotes, but compare the present invention and still have larger gap, and the drag reduction time differs greatly in the present invention, there is no long-term drag-reduction effect of the present invention.
The above, be only preferred embodiment of the present invention, is not the present invention to be done to the restriction of other form, and any those skilled in the art may utilize the technology contents of above-mentioned announcement to be changed or be modified as the equivalent embodiment of equivalent variations.But every technical solution of the present invention content that do not depart from, any simple modification, equivalent variations and the remodeling above embodiment done according to technical spirit of the present invention, still belong to the protection domain of technical solution of the present invention.
Claims (9)
1. slippery water water blanket transmits a preparation technology for flow improver mutually, it is characterized in that, concrete technology step is:
(1) acrylamide is synthetic: vinyl cyanide and water are mixed according to volume ratio 1:6.5 ~ 7.5, then add Lei Nitong, carry out hydration reaction generate the acrylamide solution that mass concentration is 15.5% ~ 20.5% at 78 ~ 140 ℃;
(2) acrylamide is concentrated: the acrylamide solution that is 15.5% ~ 20.5% by mass concentration is by the concentrated acrylamide monomer aqueous solution that obtains mass concentration 35% ~ 45%, and in the acrylamide monomer aqueous solution after concentrating, content of copper ion is controlled at below 5 ppm;
(3) preparation monomer: it is 18.5 ~ 25.5% that the acrylamide monomer aqueous solution of mass concentration 35% ~ 45% is diluted with water to mass concentration, and add the N-tert-butyl acrylamide that accounts for acrylamide monomer aqueous solution weight 0.2 ~ 2.0% to prepare mixed solution, mixed solution is cooled to 7 ~ 10 ℃, stirs;
(4) preparation reaction solution: add sodium carbonate or sodium carbonate solution to form reaction solution in the mixed solution of step (3), wherein the clean quality of sodium carbonate accounts for 2.5 ~ 8.0% of reaction solution quality, then accounts for reaction solution quality 20 ~ 100ppm sequestrant, 10 ~ 100ppm chain-transfer agent, 30 ~ 300ppm chain propagation agent and 50 ~ 250ppm water-soluble azo compounds to adding in reaction solution;
(5) polymerization, hydrolysis: in reaction unit, lead to nitrogen deoxygenation and control reacting liquid temperature at 5 ~ 15 ℃, then add and account for the reductive agent of reaction solution quality 10 ~ 120ppm and the oxygenant of 10 ~ 120ppm, 10 ~ 15 ℃ of polymerizations 1 ~ 4 hour, then be warming up to 75 ~ 85 ℃ of hydrolysis 3 ~ 6 hours, after hydrolysis, obtain blob of viscose;
(6) powder process: blob of viscose cutting, thin granulation drying treatment are obtained to polyacrylamide particle, then polyacrylamide particle is crushed and screened and obtains polyacrylamide powder; Polyacrylamide powder and sodium chloride particle are fully mixed and obtain flow improver, and wherein polyacrylamide accounts for 25 ~ 75% of flow improver weight.
2. slippery water water blanket according to claim 1 transmits the preparation technology of flow improver mutually, it is characterized in that: before vinyl cyanide described in step (1) and water mix, vinyl cyanide need carry out distilation at 78 ~ 95 ℃, and it is standby that gas phase obtains fine propylene nitrile through condensation; Water need to be preheated to 80 ℃.
3. slippery water water blanket according to claim 1 transmits the preparation technology of flow improver mutually, it is characterized in that: the simmer down to flash distillation concentrate described in step (2).
4. slippery water water blanket according to claim 1 transmits the preparation technology of flow improver mutually, it is characterized in that: Si Ban-40 that are evenly mixed with 20 ~ 500ppm in the sodium carbonate solution described in step (4).
5. slippery water water blanket according to claim 1 transmits the preparation technology of flow improver mutually, it is characterized in that: the sequestrant in step (4) is disodium ethylene diamine tetraacetate, chain-transfer agent is sodium acetate, chain propagation agent is Tetramethyl Ethylene Diamine, and water-soluble azo compounds is azo-bis-isobutyrate hydrochloride.
6. slippery water water blanket according to claim 1 transmits the preparation technology of flow improver mutually, it is characterized in that: the reductive agent described in step (5) is sodium bisulfite, and oxygenant is Potassium Persulphate.
7. slippery water water blanket according to claim 1 transmits the preparation technology of flow improver mutually, it is characterized in that: the concrete steps to logical nitrogen deoxygenation in reaction unit described in step (5) are for adding logical nitrogen 30min ~ 45min before reductive agent and oxygenant, lead to again nitrogen 5 ~ 15min after adding reductive agent and oxygenant; Make oxygen content < 200ppb in system.
8. slippery water water blanket according to claim 1 transmits the preparation technology of flow improver mutually, it is characterized in that: the particle diameter of the polyacrylamide particle described in step (6) is 3 ~ 5mm; The particle diameter of polyacrylamide powder is 40 ~ 200 orders.
9. slippery water water blanket according to claim 1 transmits the preparation technology of flow improver mutually, it is characterized in that: the concrete steps of drying treatment described in step (6) are for first dry at 85 ~ 110 ℃ with revolution percolation machine, then dry at 95 ℃ ~ 140 ℃ with vibration vulcanization bed.
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| CN112410013A (en) * | 2020-10-15 | 2021-02-26 | 德仕能源科技集团股份有限公司 | Suspension liquid drag reducer and preparation method and application thereof |
| CN114395057A (en) * | 2022-01-18 | 2022-04-26 | 中国石油大学(北京) | Polyacrylamide containing chelating sites, chelating type variable-viscosity slickwater and preparation |
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| JPH0466127A (en) * | 1990-07-03 | 1992-03-02 | Showa Denko Kk | Renewal process of catalyst |
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