CN102477124A - Preparation technology for improving intrinsic viscosity and conversion rate of acid thickener - Google Patents
Preparation technology for improving intrinsic viscosity and conversion rate of acid thickener Download PDFInfo
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- CN102477124A CN102477124A CN2010105674483A CN201010567448A CN102477124A CN 102477124 A CN102477124 A CN 102477124A CN 2010105674483 A CN2010105674483 A CN 2010105674483A CN 201010567448 A CN201010567448 A CN 201010567448A CN 102477124 A CN102477124 A CN 102477124A
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Abstract
The invention discloses a preparation technology for improving the intrinsic viscosity and conversion rate of an acid thickener. The preparation technology comprises: hydrolyzing maleic anhydride, adding an ethylene diamine tetraacetic acid solution, adding 2-methyl-2-acrylamide propanesulfonic acid and an acrylamide solution, adjusting the pH value, introducing nitrogen and adding an ammonium persulfate solution, continuing introducing nitrogen and adding 2-methyl-2-acrylamide propanesulfonic acid and an acrylamide solution for reaction, thus obtaining an acid thickener, with the pH value of the reaction system controlled at 6.8-7.2, and the reaction temperature controlled at 50DEG C-60DEG C. By controlling the pH value of the reaction system and the reaction temperature, the technology of the invention improves the intrinsic viscosity and preparation efficiency of the acid thickener, thus enhancing the integral performance of the acid thickener and reducing the preparation cost of the acid thickener.
Description
Technical field
The present invention relates to a kind of preparation technology, specifically be meant a kind of preparation technology who improves gelling agent for acid fluid intrinsic viscosity and transformation efficiency.
Background technology
Viscosifying agent is as the key of preparation gelled acid.Along with to the intensification of viscosifying agent understanding and the continuous expansion of gelled acid technology rig-site utilization, gelling agent for acid fluid is had higher requirement.Think that at present more satisfactory gelling agent for acid fluid should possess the requirement of the following aspects:
(1) soluble in water and sour, dissolution rate is than very fast;
(2) acidproof ability is better, and it is less influenced by acid concentration to the tackifying of acid;
(3) thermostability is relatively good;
(4) with other acid additive, good like compatiblenesies such as Fe stabilizer, corrosion inhibitors for acidic media;
(5) gelled acid of preparation 20%HCl, AV＞50mPas;
(6) receive the influence of mechanical shearing less;
(7) the residual sour viscosity＜10mPas of gelled acid of preparation, residue content＜7%;
(8) compare resistance-reducing yield＞50% in the pit shaft with clear water;
(9) folk prescription cost＜1000 yuan of preparation gelled acid.
The research of external gelling agent for acid fluid starts from the seventies in 20th century, has experienced the research of preparation from the natural polymer to the synthetics, and the external in recent years type kind development to gelling agent for acid fluid tends towards stability, and more pays attention to the improvement of product performance.No matter be the improvement old product or develop new product, general all attention concentrate on the high-temperature stability that improves product, filtrate-loss control, in high concentrated acid suitability and resisting high-concentration ion, anti-high shear rate, do not generate aspect such as noxious residue.
The gelling agent for acid fluid of external immediate development does not have new breakthrough on big classification, this mainly is that the material choice aspect does not have due to the breakthrough.The middle used synthetic viscosifying agent raw material of hot hole is main with acrylic amide and polyvinyls still; This type viscosifying agent has the unrivaled advantage of natural goods; On kind quantity and range of application, have overwhelming superiority, wherein especially with the tool advantage of acrylamide copolymer.The raw material of the used natural goods viscosifying agent of low temperature shallow well or middle-deep well is a host with guanidine glue, Mierocrystalline cellulose still, generally under temperature condition below 60 ℃, uses, and also only reaches about 70 ℃ through modification, because the high temperature acid resistance is undesirable, its practical application is restricted.
External most gelling agent for acid fluid product is a dry powder, is convenient to packed and transported, and also Yin Qiyi is scattered in the acid solution and is easy to use, but the emulsion-type viscosifying agent more is soluble in acid solution, thereby can improve result of use.And, produce the emulsion-type viscosifying agent and also can save production pulvis energy consumption, so, multiple emulsion-type viscosifying agent had appearred in recent years.
China starts from introduction U.S. Halliburton Company viscosifying agent in 1984 after the construction of Sichuan to the experimental study of gelling agent for acid fluid.Beginning ten surplus year in, be engaged in this work and develop product have only two families: oiling institute of Beijing oil scientific research institute and Sichuan petroleum office sky grind institute.
The gelling agent for acid fluid RTA that Beijing oiling is developed contains the monomeric multipolymer of NaAMPS (2-acrylamido-2-methyl propane sulfonic acid sodium).The gelled acid of joining 15% concentration with 0.5%RAT constant temperature 8h and all do not have deposition in 1 hour under 100 ℃ of temperature condition at 120 ℃ of following constant temperature.Institute joins gelled acid concentration and can reach 28%.It is the milk sap product that the CT1-6 gelling agent for acid fluid of being developed grinds in the sky in Sichuan petroleum office; Industry standard SY/T5694-95 (gelling agent for acid fluid CT1-6 is used in acidifying) according to its product performance establishment shows; Gelling agent for acid fluid CT1-6 in containing 20% hydrochloric acid soln of promoting agent the needed time of homodisperse less than 2h; The acid liquid viscosity of gelled acid under 93 ℃ of preparation is greater than 20mPas, and the acid liquid viscosity under 40 ℃ is greater than 26mPas.CT1-6 is the domestic gelling agent for acid fluid product that is applied at the scene the earliest of development voluntarily.
The later stage nineties 20th century; Beijing Scientific Research Institute of Petroleum Exploration and Development Planning develops cationic powdery gelling agent for acid fluid VY-101; The laboratory performance evaluation test shows; The VY-101 gelling agent for acid fluid has good tackifying, thermostability and shear resistant, and certain effect that prevents clay swelling is arranged.Rig-site utilization was carried out in this agent in the exploitation of Dagang Oilfield buried hill oil pool, owing to be the powdered macromolecule product, need take a long time during on-the-spot the preparation and dissolve.
Mostly the gelling agent for acid fluid of domestic present development is synthetic high molecular polymer product; And acrylamide copolymer is in the great majority; Mainly be because external this series products exploitation more, but the experience for reference of rich is arranged, it is bigger to develop high-level product chance.
Because the performance of natural polymer is undesirable, its practical application is restricted, and consumption also reduces relatively; Though being carried out modification, natural polymer can improve its performance to a certain extent.But synthetic polymer class viscosifying agent can improve the heat-resisting property and the anti-salt property of viscosifying agent, and therefore developing synthetic polymer has exigence, and this also is the focus of studying both at home and abroad at present.Copolymerization to monomeric purity requirement than higher, so before reacting, need purify to the monomer that is about to participate in reaction.The purpose of purifying is to remove the stopper and some impurity monomers that is mixed with in the starting monomer, in order to avoid because the existence of these impurity exerts an adverse impact to polyreaction, make polymerization product not reach expected effect.
In the preparation process of gelling agent for acid fluid; PH value of reaction system is very big to the intrinsic viscosity influence of gelling agent for acid fluid; And temperature of reaction is very big to the transformation efficiency influence of gelling agent for acid fluid; So the selection of pH value of reaction system and temperature of reaction will directly influence the overall performance and the preparation efficiency of gelling agent for acid fluid, how select a suitable pH value of reaction system and temperature of reaction that the preparation technology of gelling agent for acid fluid is seemed particularly important.
Summary of the invention
Deficiency and the defective of the object of the invention in order to overcome prior art; A kind of preparation technology who improves gelling agent for acid fluid intrinsic viscosity and transformation efficiency is provided; This preparation technology's preparation is through control pH value of reaction system and temperature of reaction; Thereby improved the intrinsic viscosity and the preparation efficiency of gelling agent for acid fluid, and then improved the overall performance of gelling agent for acid fluid, reduced the manufacturing cost of gelling agent for acid fluid.
The object of the invention is realized through following technical proposals: a kind of preparation technology who improves gelling agent for acid fluid intrinsic viscosity and transformation efficiency may further comprise the steps:
(a) take by weighing MALEIC ANHYDRIDE and put into container and be hydrolyzed, after the hydrolysis container is put into thermostat(t)ed water and be incubated;
(b) in the MALEIC ANHYDRIDE container, add edta solution as complexing agent, and then add 2-methyl-2-acrylamido propanesulfonic acid and acrylamide soln;
(c) regulate the pH value in the container with 10% sodium hydroxide solution;
(d) logical nitrogen deoxygenation and stirring the back and adds ammonium persulfate solution;
(e) continue logical nitrogen, the conditioned reaction temperature adds methyl-2-acrylamido propanesulfonic acid and acrylamide soln again, promptly obtains gelling agent for acid fluid after the reaction.
The pH value transfers to 6.8～7.2 in the said step (c).
The pH value of reaction system transfers to 7.0 in the said step (c).
Churning time is 15 minutes in the said step (d).
Conditioned reaction temperature to 50 ℃ in the said step (e)～60 ℃,
Temperature of reaction transfers to 55 ℃ in the said step (e).
The reaction times is 7 hours in the said step (e).
In sum; The invention has the beneficial effects as follows: through control pH value of reaction system and temperature of reaction; Thereby improved the intrinsic viscosity and the preparation efficiency of gelling agent for acid fluid, and then improved the overall performance of gelling agent for acid fluid, reduced the manufacturing cost of gelling agent for acid fluid.
Embodiment
Below in conjunction with embodiment, the present invention is done detailed description further, but embodiment of the present invention is not limited thereto.
Embodiment:
The present invention relates to a kind of preparation technology who improves gelling agent for acid fluid intrinsic viscosity and transformation efficiency, may further comprise the steps:
(a) take by weighing MALEIC ANHYDRIDE and put into container and be hydrolyzed, after the hydrolysis container is put into thermostat(t)ed water and be incubated;
(b) in the MALEIC ANHYDRIDE container, add edta solution as complexing agent, and then add 2-methyl-2-acrylamido propanesulfonic acid and acrylamide soln;
(c) regulate the pH value in the container with 10% sodium hydroxide solution;
(d) logical nitrogen deoxygenation and stirring the back and adds ammonium persulfate solution;
(e) continue logical nitrogen, the conditioned reaction temperature adds methyl-2-acrylamido propanesulfonic acid and acrylamide soln again, promptly obtains gelling agent for acid fluid after the reaction.
The pH value transfers to 6.8～7.2 in the said step (c).
The pH value of reaction system transfers to 7.0 in the said step (c).
Churning time is 15 minutes in the said step (d).
Conditioned reaction temperature to 50 ℃ in the said step (e)～60 ℃,
Temperature of reaction transfers to 55 ℃ in the said step (e).
The reaction times is 7 hours in the said step (e).
For the influence to the gelling agent for acid fluid intrinsic viscosity of the pH value of investigating solution, the present invention transfers to different pH values with reaction system with NaOH solution, and the gelling agent for acid fluid intrinsic viscosity of preparation is as shown in the table:
| The pH value | 6.4 | 6.6 | 6.8 | 7.0 | 7.2 | 7.4 | 7.6 |
| Intrinsic viscosity (ml/g) | 414 | 512 | 624 | 650 | 629 | 526 | 421 |
Can find out that through last table the pH value is in 6.4～7.0 scope, along with the increase of pH value; The gelling agent for acid fluid intrinsic viscosity obviously increases, and when pH value of reaction system increased to 7.0, it is maximum that the intrinsic viscosity value reaches; Continue the augmenting response system pH, the gelling agent for acid fluid intrinsic viscosity begins to descend.So in order to obtain higher gelling agent for acid fluid intrinsic viscosity, pH value of reaction system should be controlled between 6.8～7.2, and preferentially is chosen as neutrallty condition, promptly pH value of reaction system is 7.0.
Because temperature of reaction is very big to the influence of the transformation efficiency among the gelling agent for acid fluid preparation technology, reason is: along with the increase of temperature of reaction, the rate of decomposition of initiator increases; Polymerization rate is accelerated, and monomer conversion is high, and after reaction reaches certain temperature; Monomer conversion changes little, but temperature of reaction is too high, and the radical number of generation increases; Can cause the polymerization degree to reduce, molecular weight of product reduces, but the polymeric reaction temperature bottom line should be more than the temperature of decomposition of initiator.In order to obtain best temperature of reaction, the present invention transfers to different numerical value with temperature of reaction, and the gelling agent for acid fluid transformation efficiency of preparation is as shown in the table:
| Temperature of reaction (℃) | 35 | 40 | 45 | 50 | 55 | 60 | 65 |
| Transformation efficiency (%) | 81 | 85 | 92 | 97 | 93 | 86 | 82 |
Can find out that from last table temperature of reaction is in 35 ℃～40 ℃ low scope, the rate of decomposition of initiator is slower, and the quantity of radical has a lot of monomers can not participate in polymerization with active low, and transformation efficiency is lower, and the molecular weight of polymkeric substance is also low; Along with temperature is elevated in 50 ℃ the process by 40 ℃ gradually, the decomposition rate of initiator is obviously accelerated, and the quantity of radical and activity all increase to some extent; Extent of polymerization uprises; Thereby also rising rapidly of transformation efficiency, when at 50 ℃, it is maximum that the gelling agent for acid fluid transformation efficiency reaches.But when temperature continues to increase by 50 ℃; The gelling agent for acid fluid transformation efficiency descends on the contrary; This is because under too high temperature; A large amount of initiator generation thermolysis and produce a large amount of radicals rapidly and cause combination, the chain termination speed increasing degree that makes polymerization system is greatly to the increasing degree much larger than rate of chain growth.In addition, owing to the square root with closely-related kinetic chain length of polymericular weight and number of free radical is inversely proportional to, be directly proportional with rate of polymerization, the rising of temperature will cause the gelling agent for acid fluid transformation efficiency to reduce.Therefore, in order to obtain high molecular weight polymers, it is in 45 ℃～55 ℃ the scope that temperature of reaction should be controlled at, and preferentially is chosen as 50 ℃.
As stated, just can realize the present invention preferably.
Claims (7)
1. a preparation technology who improves gelling agent for acid fluid intrinsic viscosity and transformation efficiency is characterized in that, may further comprise the steps:
(a) take by weighing MALEIC ANHYDRIDE and put into container and be hydrolyzed, after the hydrolysis container is put into thermostat(t)ed water and be incubated;
(b) in the MALEIC ANHYDRIDE container, add edta solution as complexing agent, and then add 2-methyl-2-acrylamido propanesulfonic acid and acrylamide soln;
(c) regulate the pH value in the container with 10% sodium hydroxide solution;
(d) logical nitrogen deoxygenation and stirring the back and adds ammonium persulfate solution;
(e) continue logical nitrogen, the conditioned reaction temperature adds methyl-2-acrylamido propanesulfonic acid and acrylamide soln again, promptly obtains gelling agent for acid fluid after the reaction.
2. a kind of preparation technology who improves gelling agent for acid fluid intrinsic viscosity and transformation efficiency according to claim 1 is characterized in that, the pH value transfers to 6.8～7.2 in the said step (c).
3. a kind of preparation technology who improves gelling agent for acid fluid intrinsic viscosity and transformation efficiency according to claim 2 is characterized in that, the pH value of reaction system transfers to 7.0 in the said step (c).
4. a kind of preparation technology who improves gelling agent for acid fluid intrinsic viscosity and transformation efficiency according to claim 1 is characterized in that, churning time is 15 minutes in the said step (d).
5. a kind of preparation technology who improves gelling agent for acid fluid intrinsic viscosity and transformation efficiency according to claim 1 is characterized in that, conditioned reaction temperature to 50 ℃ in the said step (e)～60 ℃,
6. a kind of preparation technology who improves gelling agent for acid fluid intrinsic viscosity and transformation efficiency according to claim 5 is characterized in that, temperature of reaction transfers to 55 ℃ in the said step (e).
7. a kind of preparation technology who improves gelling agent for acid fluid intrinsic viscosity and transformation efficiency according to claim 1 is characterized in that, the reaction times is 7 hours in the said step (e).
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105777984A (en) * | 2016-05-17 | 2016-07-20 | 山东大学 | Temperature-resistant and salt-tolerant bittern pipeline drag reducer and preparation method thereof |
| CN106188392A (en) * | 2016-07-18 | 2016-12-07 | 河南弘康环保科技有限公司 | A kind of ternary polymerization anion-polyacrylamide and preparation method thereof |
-
2010
- 2010-11-22 CN CN2010105674483A patent/CN102477124A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105777984A (en) * | 2016-05-17 | 2016-07-20 | 山东大学 | Temperature-resistant and salt-tolerant bittern pipeline drag reducer and preparation method thereof |
| CN106188392A (en) * | 2016-07-18 | 2016-12-07 | 河南弘康环保科技有限公司 | A kind of ternary polymerization anion-polyacrylamide and preparation method thereof |
| CN106188392B (en) * | 2016-07-18 | 2018-05-11 | 河南弘康环保科技有限公司 | A kind of ternary polymerization anion-polyacrylamide and preparation method thereof |
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Application publication date: 20120530 |