CN111621268A - High-temperature-resistant cross-linked polysaccharide polymer for drilling fluid and preparation method thereof - Google Patents
High-temperature-resistant cross-linked polysaccharide polymer for drilling fluid and preparation method thereof Download PDFInfo
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- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/70—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the isocyanates or isothiocyanates used
- C08G18/72—Polyisocyanates or polyisothiocyanates
- C08G18/74—Polyisocyanates or polyisothiocyanates cyclic
- C08G18/75—Polyisocyanates or polyisothiocyanates cyclic cycloaliphatic
- C08G18/751—Polyisocyanates or polyisothiocyanates cyclic cycloaliphatic containing only one cycloaliphatic ring
- C08G18/752—Polyisocyanates or polyisothiocyanates cyclic cycloaliphatic containing only one cycloaliphatic ring containing at least one isocyanate or isothiocyanate group linked to the cycloaliphatic ring by means of an aliphatic group
- C08G18/753—Polyisocyanates or polyisothiocyanates cyclic cycloaliphatic containing only one cycloaliphatic ring containing at least one isocyanate or isothiocyanate group linked to the cycloaliphatic ring by means of an aliphatic group containing one isocyanate or isothiocyanate group linked to the cycloaliphatic ring by means of an aliphatic group having a primary carbon atom next to the isocyanate or isothiocyanate group
- C08G18/755—Polyisocyanates or polyisothiocyanates cyclic cycloaliphatic containing only one cycloaliphatic ring containing at least one isocyanate or isothiocyanate group linked to the cycloaliphatic ring by means of an aliphatic group containing one isocyanate or isothiocyanate group linked to the cycloaliphatic ring by means of an aliphatic group having a primary carbon atom next to the isocyanate or isothiocyanate group and at least one isocyanate or isothiocyanate group linked to a secondary carbon atom of the cycloaliphatic ring, e.g. isophorone diisocyanate
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- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
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- C08G18/72—Polyisocyanates or polyisothiocyanates
- C08G18/74—Polyisocyanates or polyisothiocyanates cyclic
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- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/70—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the isocyanates or isothiocyanates used
- C08G18/72—Polyisocyanates or polyisothiocyanates
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Abstract
The invention discloses a high-temperature-resistant cross-linked polysaccharide polymer for drilling fluid and a preparation method thereof, wherein the high-temperature-resistant cross-linked polysaccharide polymer for drilling fluid is prepared by chemically cross-linking a polysaccharide polymer and isocyanate in an organic solvent, and the raw material formula comprises 50-85 parts of the polysaccharide polymer, 2-10 parts of isocyanate, 0.01-0.5 part of a catalyst and 10-45 parts of the organic solvent. The high-temperature resistant cross-linked polysaccharide polymer for the drilling fluid has the advantages of good structural stability, high cross-linking density, good high-temperature resistance, filtration loss reduction, salt resistance and the like by cross-linking molecules or particles through chemical bonds, and can be used as a high-temperature resistant filtrate reducer of the drilling fluid to continuously meet the requirement on high-temperature resistance in petroleum drilling engineering.
Description
Technical Field
The invention belongs to the technical field of fluid loss agents for drilling fluids, and particularly relates to a high-temperature-resistant cross-linked polysaccharide polymer for drilling fluids and a preparation method thereof.
Background
In the process of oil and gas drilling, the drilling fluid process technology is an important component of oil and gas drilling engineering. It plays a critical role in ensuring safe, quality, and fast drilling. From the 20 th century, with the rapid development of the world oil industry, the number, speed and depth of drilled wells are remarkably increased, the drilled formations are more complex, and the open holes are longer and longer, so that higher requirements on drilling fluids are provided.
Along with the increase of the current drilling depth, the drilling operation is increasingly complicated, and the wide application of the technologies of directional wells, horizontal wells, multi-lateral wells, multilateral wells and the like has higher and higher requirements on the temperature resistance, salt resistance, cutting improvement and other performances of the drilling fluid treating agent. Although the oil-based drilling fluid has the advantages of high temperature resistance, good lubricating property and the like, the oil-based drilling fluid is relatively rarely applied due to the factors of cost, environment, safety, cognition and the like in China. Therefore, high temperature resistant water-based drilling fluid systems will remain the focus of future drilling fluid technology, and one of the key points of high temperature water-based drilling fluid systems is to have a high temperature and salt contamination resistant treatment agent.
The starch natural polymer has rich source, low price, easy biodegradation, environmental protection and no toxicity, is widely used in the petroleum industry, is one of the earliest drilling fluid filtrate reducer, mainly has the functions of reducing filtration loss, tackifying, stabilizing well walls, preventing collapse and the like, can be used in fresh water, seawater and saturated salt water drilling fluid, has better effect particularly in the saturated salt water drilling fluid, but is easy to decompose and ferment at high temperature, thereby seriously limiting the application of the starch.
The property of the natural starch is changed by physical, chemical or enzymatic means, and the starch derivative, namely modified starch with changed, enhanced or new property can be prepared by cutting, rearranging and oxidizing molecules or introducing substituent groups into starch molecules so as to continuously improve and enhance the high temperature resistance and the fluid loss reducing effect of the starch. The modified starch DFD-140 for the drilling fluid has the advantages that the high-temperature resistance modified group is introduced into the molecular chain, so that the temperature resistance and salt resistance of the modified starch DFD-140 are improved, and the modified starch DFD-140 can resist about 140 ℃ at most. Chinese invention patent with publication number CN106336859A (published Japanese 2008-09-03) discloses a temperature resistant starch composition for drilling fluid and a preparation method thereof, which is prepared by starch, a catalyst, a cationic reagent and a cross-linking agent in a specific process; the cross-linked starch for drilling fluid disclosed in Chinese patent No. ZL201410840646.0 (published Japanese 2015-04-29) is prepared by esterifying starch and organic phosphonate in organic solvent in the presence of buffer solution, reacting with sodium chloroacetate under alkaline condition, and performing cross-linking reaction under the action of initiator and cross-linking agent; chinese patent No. ZL200910242693.4 published 2010-06-16) discloses a high temperature resistant and saturated salt resistant fluid loss additive prepared by reacting modified starch, polyacrylonitrile hydrolysate, propylene sulfonate and an initiator, wherein the high temperature resistant performance of the starch is improved by crosslinking modification or introduction of high temperature resistant groups to the starch, the highest resistance can be about 140 ℃, and the requirement of deep well in oil drilling on high temperature resistant performance (above 150 ℃) still cannot be met.
Disclosure of Invention
Aiming at the defects in the prior art, the invention aims to provide the high-temperature-resistant cross-linked polysaccharide polymer for the drilling fluid, which is cross-linked by chemical bonds, has good structural stability and high cross-linking density, and has the advantages of good high temperature resistance, filtration loss reduction, salt resistance and the like.
The invention also aims to provide a preparation method of the high-temperature-resistant cross-linked polysaccharide polymer for the drilling fluid, which has the advantages of wide raw material source, moderate cost, controllable reaction and large-scale production.
In order to achieve the above purposes, the invention adopts the technical scheme that: a high temperature resistant polysaccharide polymer for drilling fluid is prepared by chemically crosslinking hydroxyl on a polysaccharide polymer molecular structure and NCO of isocyanate in an organic solvent, and comprises the following raw materials in parts by weight:
further, the polysaccharide polymer comprises the following raw materials in parts by weight:
further, the polysaccharide polymer is one or more of cellulose and derivatives thereof, chitin, alginic acid and starch natural high molecular materials.
Further, the isocyanate is one or more of toluene diisocyanate, diphenylmethane diisocyanate and isophorone diisocyanate.
Furthermore, the catalyst is one or more of organic tin, organic zinc and organic bismuth organometallic compounds.
Further, the organic solvent is a polar solvent and is one or more of butyl acetate, ethyl acetate, cyclohexanone and tetrahydrofuran.
The invention provides a preparation method of a high-temperature-resistant cross-linked polysaccharide polymer for drilling fluid, which comprises the following steps:
(1) vacuum drying polysaccharide polymer;
(2) adding a polysaccharide polymer and an organic solvent into a reaction kettle, heating and keeping the temperature between 40 and 60 ℃, and stirring for 0.5 to 2 hours;
(3) slowly adding isocyanate, and reacting for 1-3 hours at a high speed under the condition of 60-90 ℃;
(4) adding a catalyst, and continuously reacting for 1-2 hours;
(5) distilling and recovering the organic solvent in the obtained reaction product to obtain the cross-linked polysaccharide.
Further, the method also comprises the steps of drying, crushing and sieving the cross-linked starch product obtained in the step (5) to obtain the required finished product. The crushing degree can be controlled according to actual needs to obtain the required granularity of the finished product.
The cross-linked polysaccharide polymer is used as a high-temperature-resistant fluid loss additive for drilling fluid.
The invention has the technical effects that: the high-temperature resistant polysaccharide cross-linked polymer for the drilling fluid provided by the invention has the advantages of good structure stability, high cross-linking density, good high-temperature resistance, filtration loss reduction, salt resistance and the like by cross-linking molecules or particles through chemical bonds, is suitable for a high-temperature resistant fluid loss additive of the drilling fluid, and can improve the high-temperature resistance of the cross-linked polysaccharide polymer so as to continuously meet the requirement on the high-temperature resistance in oil drilling engineering.
Drawings
FIG. 1 is a molecular structural formula of a typical polysaccharide polymer in an embodiment of the present invention.
Detailed Description
In order that those skilled in the art will better understand the technical solutions of the present invention, the present invention will be further described in detail with reference to the following detailed description. The reagents and equipment in the examples are all commercially available.
Cellulose and derivatives thereof widely existing in nature, chitin, alginic acid, starch and other natural high polymer materials belong to natural polysaccharide polymers, the sources are wider, and the molecular structures of the natural high polymer materials contain a large amount of hydroxyl groups. Therefore, the invention utilizes the hydroxyl on the molecular structure of the polysaccharide polymer shown in figure 1 to react with NCO of isocyanate to carry out chemical crosslinking on the molecules or particles of the polysaccharide polymer, easily prepares the crosslinked polysaccharide polymer with high crosslinking density, has stable structure, adjustable and controllable crosslinking degree, has the advantages of better high temperature resistance, filtration loss reduction, salt resistance and the like, is suitable for a high temperature resistant fluid loss additive of drilling fluid, can improve the high temperature resistance of the crosslinked polysaccharide polymer, and continuously meets the requirement of high temperature resistance in oil drilling engineering.
Example 1
The embodiment provides a high-temperature-resistant cross-linked polysaccharide polymer for drilling fluid, which comprises the following raw materials in parts by weight: 68kg of polysaccharide polymer (pregelatinized starch, Hebei Henbei Hengji chemical industry), 2.2kg of isocyanate (TDI-80, a mixture of 80 mass percent of 2, 4-toluene diisocyanate and 20 mass percent of 2, 6-toluene diisocyanate, Cangzhou Dazai), 0.01kg of catalyst (organic tin, T12, United states gas chemical industry) and 29.79kg of organic solvent (butyl acetate, Shandong Noll chemical industry).
Vacuum drying polysaccharide polymer in advance for later use; adding 68kg of dried polysaccharide polymer and 29.79kg of organic solvent into a reaction kettle, heating to 50 ℃, and stirring for 1.5 hours; slowly dripping 2.2kg of isocyanate, and reacting for 1 hour at a high speed under the temperature of 90 ℃; adding 0.01kg of catalyst, and continuing to react for 2 hours; distilling the product to recover the organic solvent, and then sequentially drying, crushing and sieving by a 60-mesh standard sieve to obtain the product.
Example 2
The embodiment provides a high-temperature-resistant cross-linked polysaccharide polymer for drilling fluid, which comprises the following raw materials in parts by weight: 50kg of polysaccharide polymer 1 (pregelatinized starch, Hebei chemostat), 34.8kg of polysaccharide polymer 2 (carboxymethyl starch, Shandong Weifang Litte), 5kg of isocyanate (MDI-50, a mixture of 50% by mass of 2, 4-diphenylmethane diisocyanate and 50% by mass of 4, 4' -diphenylmethane diisocyanate, Vanhua Chemicals), 0.2kg of catalyst (organic zinc, Bicat Z, Shanghai Denton Chemicals) and 10kg of organic solvent (tetrahydrofuran, Shandong Nool chemical).
Pre-vacuum drying polysaccharide polymer 1 and polysaccharide polymer 2 for later use; adding 50kg of dried polysaccharide polymer 1, 34.8kg of polysaccharide polymer 2 and 10kg of organic solvent into a reaction kettle, heating to 50 ℃, and stirring for 0.5 hour; slowly dripping 5kg of isocyanate, and reacting for 2 hours at 80 ℃ by high-speed stirring; adding 0.2kg of catalyst, and continuously stirring for reaction for 1 hour; distilling the product to recover the organic solvent, and then sequentially drying, crushing and sieving by a 60-mesh standard sieve to obtain the product.
Example 3
The embodiment provides a high-temperature-resistant cross-linked polysaccharide polymer for drilling fluid, which comprises the following raw materials in parts by weight: 50kg of polysaccharide polymer 1 (pregelatinized starch, Hebei Hecheng polymerization chemical), 25kg of polysaccharide polymer 2 (carboxymethyl cellulose, LV-CMC), 7kg of isocyanate (IPDI, isophorone diisocyanate, Corsika), 0.5kg of catalyst (organic bismuth, Bicat8118, American advanced chemical), and 17.5kg of organic solvent (methyl ethyl ketone, Guangdong blue arrow chemical).
Pre-vacuum drying polysaccharide polymer 1 and polysaccharide polymer 2 for later use; adding 50kg of dried polysaccharide polymer 1, 25kg of polysaccharide polymer 2 and 17.5kg of organic solvent into a reaction kettle, heating to 40 ℃, and stirring for 2 hours; slowly dropwise adding 7kg of isocyanate, and reacting for 3 hours at 60 ℃ by high-speed stirring; adding 0.5kg of catalyst, and continuously stirring for reaction for 1 hour; distilling the product to recover the organic solvent, and then sequentially drying, crushing and sieving by a 60-mesh standard sieve to obtain the product.
Example 4
The embodiment provides a high-temperature-resistant cross-linked polysaccharide polymer for drilling fluid, which comprises the following raw materials in parts by weight: 84kg of polysaccharide polymer (pregelatinized starch, Hebei Henbei Hengji chemical industry), 6kg of isocyanate 1(MDI-50, Wanhua chemical industry), 3.8kg of isocyanate 2(TDI-80, Cangzhou Daghua), 0.2kg of catalyst (bismuth-zinc composite catalyst, bismuth-zinc isooctanoate, American PIMM) and 6.0kg of organic solvent (butyl acetate, Shandong Noll chemical industry).
Vacuum drying polysaccharide polymer in advance for later use; adding 84kg of dried polysaccharide polymer and 6.0kg of organic solvent into a reaction kettle, heating to 60 ℃, and stirring for 1 hour; slowly dripping 9.8kg of isocyanate, and reacting for 2 hours at a high speed at the temperature of 70 ℃; adding 0.2kg of catalyst, and continuously stirring for reaction for 2 hours; distilling the product to recover the organic solvent, and then sequentially drying, crushing and sieving by a 60-mesh standard sieve to obtain the product.
Example 5
The embodiment provides a high-temperature-resistant cross-linked polysaccharide polymer for drilling fluid, which comprises the following raw materials in parts by weight: 53.48kg of polysaccharide polymer (pregelatinized starch, Hebei Henbei Hengji chemical industry), 1.5kg of isocyanate (TDI-80, Cangzhou Daghua), 0.02kg of catalyst (organic tin, T12, American gas chemical industry) and 45kg of organic solvent (butyl acetate, Shandong Noll chemical industry).
Vacuum drying polysaccharide polymer in advance for later use; 53.48kg of dried polysaccharide polymer and 45kg of organic solvent are added into a reaction kettle, heated to 50 ℃, and stirred for 1.5 hours; slowly dripping 1.5kg of isocyanate, and reacting for 1.5 hours at a high speed under stirring at the temperature of 80 ℃; adding 0.02kg of catalyst, and continuing to react for 2 hours; distilling the product to recover the organic solvent, and then sequentially drying, crushing and sieving by a 60-mesh standard sieve to obtain the product.
The products obtained in examples 1 to 5 were evaluated for viscosity, temperature resistance, salt resistance, and fluid loss reduction according to the drilling fluid-related standards and testing methods, and the properties are shown in table 1:
note: the addition of the cross-linked polysaccharide polymer is 15g/L, and the curing is carried out for 16h at 160 DEG C
Therefore, the products provided by the examples 1 to 5 are polysaccharide polymers highly crosslinked through chemical bonds, have excellent high temperature resistance and salt resistance, have low filtration loss and are suitable for deepwater high-temperature drilling engineering.
It will be apparent to those skilled in the art that various changes and modifications may be made in the present invention without departing from the spirit and scope of the invention. Thus, if such modifications and variations of the present invention fall within the scope of the claims of the present invention and their equivalents, the present invention is intended to include such modifications and variations.
Claims (9)
1. The high-temperature-resistant cross-linked polysaccharide polymer for the drilling fluid is characterized by being prepared by chemically cross-linking hydroxyl on a molecular structure of the polysaccharide polymer and NCO of isocyanate in an organic solvent, and comprising the following raw materials in parts by weight:
2. the high-temperature-resistant cross-linked polysaccharide polymer for the drilling fluid is characterized by comprising the following raw materials in parts by mass:
3. the high temperature cross-linking resistant polysaccharide polymer for drilling fluid according to claim 1, wherein the polysaccharide polymer is one or more of cellulose and derivatives thereof, chitin, alginic acid and starch natural polymer materials.
4. The high temperature resistant cross-linked polysaccharide polymer for drilling fluid of claim 1, wherein the isocyanate is one or more of toluene diisocyanate, diphenylmethane diisocyanate, and isophorone diisocyanate.
5. The high temperature resistant cross-linked polysaccharide polymer for drilling fluid of claim 1, 2, 3 or 4, wherein the catalyst is one or more of organic tin, organic zinc and organic bismuth organometallic compounds.
6. The high temperature resistant cross-linked polysaccharide polymer for drilling fluid of claim 5, wherein the organic solvent is a polar solvent selected from one or more of butyl acetate, ethyl acetate, cyclohexanone and tetrahydrofuran.
7. The method for preparing the high-temperature resistant cross-linked polysaccharide polymer for the drilling fluid, which is disclosed by claims 1 to 6, comprises the following steps:
(1) drying polysaccharide polymer in advance for later use;
(2) adding a polysaccharide polymer and an organic solvent into a reaction kettle, heating and keeping the temperature between 40 and 60 ℃, and stirring for 0.5 to 2 hours;
(3) slowly dropwise adding isocyanate, and reacting for 1-3 hours at a high speed under the condition of 60-90 ℃;
(4) adding a catalyst, and continuously reacting for 0.5-2 hours;
(5) distilling and recovering the organic solvent in the obtained reaction product to obtain the cross-linked polysaccharide polymer product.
8. The method according to claim 7, wherein the cross-linked polysaccharide polymer obtained in step (5) is dried and pulverized to obtain the desired product.
9. The cross-linked polysaccharide polymer of claims 1 to 6 for use in a drilling fluid high temperature fluid loss additive.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20050003966A1 (en) * | 2003-04-11 | 2005-01-06 | Dobson James W. | Method of increasing the low shear rate viscosity of well drilling and servicing fluids containing calcined magnesia bridging solids, the fluids and methods of use |
| GB2444158A (en) * | 2005-01-11 | 2008-05-28 | Schlumberger Holdings | Polymer viscosifying agent for wellbore fluids |
| WO2014154348A1 (en) * | 2013-03-25 | 2014-10-02 | Borregaard As | Composition comprising water-soluble polymer and microfibrillated cellulose, product and method for oilfield applications |
| US20180127638A1 (en) * | 2016-11-07 | 2018-05-10 | Covestro Llc | Time released delivery of functional chemicals |
| CN110283575A (en) * | 2019-06-12 | 2019-09-27 | 刘国辉 | A kind of high temperature resistant salt tolerant fluid loss agent |
-
2020
- 2020-04-28 CN CN202010348964.0A patent/CN111621268A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20050003966A1 (en) * | 2003-04-11 | 2005-01-06 | Dobson James W. | Method of increasing the low shear rate viscosity of well drilling and servicing fluids containing calcined magnesia bridging solids, the fluids and methods of use |
| GB2444158A (en) * | 2005-01-11 | 2008-05-28 | Schlumberger Holdings | Polymer viscosifying agent for wellbore fluids |
| WO2014154348A1 (en) * | 2013-03-25 | 2014-10-02 | Borregaard As | Composition comprising water-soluble polymer and microfibrillated cellulose, product and method for oilfield applications |
| US20180127638A1 (en) * | 2016-11-07 | 2018-05-10 | Covestro Llc | Time released delivery of functional chemicals |
| CN110283575A (en) * | 2019-06-12 | 2019-09-27 | 刘国辉 | A kind of high temperature resistant salt tolerant fluid loss agent |
Non-Patent Citations (1)
| Title |
|---|
| 杨小玲等: "交联淀粉胶粘剂的制备及性能研究", 《中国胶粘剂》 * |
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Inventor after: Feng Liqiong Inventor after: Sun Zhongjun Inventor after: Quan Huanzhe Inventor after: Li Hongying Inventor after: Zhang Yunlei Inventor after: Zhang Yongjian Inventor before: Li Hongying Inventor before: Quan Huanzhe Inventor before: Feng Liqiong Inventor before: Zhang Yunlei Inventor before: Zhang Yongjian Inventor before: Sun Zhongjun |
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