CN110078986B - A kind of preparation method of bifunctional expanded elastomer material - Google Patents

A kind of preparation method of bifunctional expanded elastomer material Download PDF

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CN110078986B
CN110078986B CN201810077018.XA CN201810077018A CN110078986B CN 110078986 B CN110078986 B CN 110078986B CN 201810077018 A CN201810077018 A CN 201810077018A CN 110078986 B CN110078986 B CN 110078986B
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rubber
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CN110078986A (en
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张磊
杨海波
张建国
邹晓敏
李国锋
赵勇
董恩博
马明新
齐志刚
陈阳
邵茹
高辉
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Sinopec Petroleum Engineering Technical Services Co., Ltd.
China Petrochemical Corp
Sinopec Shengli Petroleum Engineering Corp
Drilling Technology Research Institute of Sinopec Shengli Petroleum Engineering Corp
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Sinopec Oilfield Service Corp
Sinopec Shengli Petroleum Engineering Corp
Drilling Technology Research Institute of Sinopec Shengli Petroleum Engineering Corp
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
    • B29B7/00—Mixing; Kneading
    • B29B7/002—Methods
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C35/00—Heating, cooling or curing, e.g. crosslinking or vulcanising; Apparatus therefor
    • B29C35/02—Heating or curing, e.g. crosslinking or vulcanizing during moulding, e.g. in a mould
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L15/00—Compositions of rubber derivatives
    • C08L15/005—Hydrogenated nitrile rubber
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2205/00—Polymer mixtures characterised by other features
    • C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
    • C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend

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Abstract

本发明公开了一种双功能膨胀弹性体材料及制备方法，其含有以下组分：氢化丁腈橡胶、膨胀组分、补强填充剂、固化剂、促进剂、分散剂、防老剂、氧化锌、氧化镁。制备方法方法，即将原料混炼；混炼后放入挤出机内挤出；最后放入硫化机中硫化成型。本发明是在橡胶基体中引入亲水亲油基团或亲水亲油组分,吸油水后可膨胀并产生较大膨胀压力；具有良好的吸水吸油性能，且本生产方法采用连续挤出硫化工艺，具有加工工序比较少、节省人力和原材料等优点，并且产品质量稳定、产量高、工效高、适应大批量生产。The invention discloses a bifunctional expanded elastomer material and a preparation method, which contains the following components: hydrogenated nitrile rubber, expansion components, reinforcing filler, curing agent, accelerator, dispersant, anti-aging agent, zinc oxide , Magnesium oxide. The preparation method comprises the following steps: kneading the raw materials; putting it into an extruder for extrusion after kneading; finally putting it into a vulcanizer for vulcanization and molding. In the present invention, hydrophilic and lipophilic groups or hydrophilic and lipophilic components are introduced into the rubber matrix, and after absorbing oil and water, it can expand and generate a large expansion pressure; it has good water and oil absorption performance, and the production method adopts continuous extrusion vulcanization. The technology has the advantages of less processing steps, saving manpower and raw materials, etc., and the product quality is stable, the output is high, the work efficiency is high, and it is suitable for mass production.

Description

Preparation method of difunctional expandable elastomer material
Technical Field
The invention relates to the field of novel functional polymer materials, in particular to a preparation method of a difunctional expanded elastomer material, which is particularly suitable for the technical field of thermal oil recovery of high-temperature and high-pressure deep wells and ultra-deep wells.
Background
The double-function expanding elastomer material is one new kind of functional polymer material, and is prepared through introducing hydrophilic group or component and lipophilic group or component into elastomer matrix, and after absorbing water and oil, the elastomer material may expand to several times or ten times its own weight or volume and produce great expansion pressure.
With the continuous deep promotion of modern industrialization process in China, the demand for oil is increasing day by day, and oil exploitation is more oriented to the midwest oil and gas fields and the offshore oil and gas fields, which also faces a more severe oil exploitation environment. Although the nitrile rubber has better oil resistance and physical and mechanical properties, the nitrile rubber has poor high temperature resistance of only 110 ℃ and 120 ℃, is easy to oxidize and has poor abrasion resistance, and sealing material products need to be replaced periodically. Therefore, the nitrile rubber does not meet the development of the traditional Chinese and western parts and offshore oil and gas fields, especially the proposal of the high-temperature high-pressure deep well and ultra-deep well thermal oil extraction technology, and a rubber sealing material with excellent high-temperature and high-pressure resistance and sealing property is needed to solve the bottleneck of the new oil extraction technology on the sealing material.
Hydrogenated nitrile rubber has been used to replace nitrile rubber in recent years abroad to overcome the defects that nitrile rubber is not high temperature resistant and is easy to oxidize. The hydrogenated nitrile rubber has good high temperature resistance, can be used in 150 ℃ oil medium, and has greatly improved oxidation resistance and physical and mechanical properties due to partial hydrogenation of double bonds in the structure. At present, the usage amount of hydrogenated nitrile rubber accounts for 20% of the usage amount of nitrile rubber, and the usage amount of hydrogenated nitrile rubber is continuously on the rising trend, and the hydrogenated nitrile rubber is considered to be one of the development directions of special rubber in the future.
But we also see that the existing expansion elastomers are all water-absorbing or oil-absorbing expansion, most of downhole liquid is oil-water mixture along with the development of oil field to the middle and later period, and the packer prepared by adopting the expansion elastomer material is required to be expanded and sealed when meeting the liquid.
Disclosure of Invention
The invention aims to solve the problems in the prior art and provides a preparation method of a difunctional expansion elastomer material which can expand and seal when meeting liquid, has simple process and low preparation cost.
The purpose of the invention is realized by the following technical scheme:
a dual function expanding elastomeric material comprising: 20-30 parts by mass of hydrogenated nitrile rubber; 3-10 parts by mass of natural rubber and/or synthetic rubber; 30-35 parts by mass of an expansion component; 8-9 parts by mass of a reinforcing filler; 2-3 parts of a curing agent; 0.4 to 1.0 mass portion of an accelerator; 2-4 parts of a dispersing agent; 0.5-1.0 part by mass of an anti-aging agent; 1.0-2.5 parts by mass of zinc oxide; 0.5 to 1.0 mass part of magnesium oxide.
Further: 20-30 parts by mass of hydrogenated nitrile rubber; 3-10 parts by mass of natural rubber and/or synthetic rubber; 30.2 to 32.8 parts by mass of an expansion component; 8.1 to 8.4 parts by mass of a reinforcing filler; 2.4 to 3.0 mass portions of curing agent; 0.4 to 1.0 mass portion of an accelerator; 2.8 to 3.9 parts by mass of a dispersant; 0.8-1.0 part by mass of an anti-aging agent; 1.2-2.3 parts by mass of zinc oxide; 0.6 to 1.0 mass part of magnesium oxide.
The synthetic rubber comprises one or a mixture of more of styrene-butadiene rubber, polyisoprene, butyl rubber, polybutadiene rubber and acrylonitrile-butadiene copolymer; the expansion component comprises modified black carbon black, high-sodium bentonite, white carbon black and polyvinyl alcohol, starch grafted acrylamide-methyl methacrylate copolymer, maleic anhydride graft, hydrophilic polyurethane prepolymer and polyacrylic acid, or comprises one or a mixture of a plurality of polyacrylic acid, polyacrylate, polyacrylamide and acrylic acid modifier; the curing agent comprises a dihydroxypolyether; the reinforcing filler comprises one or more of black carbon black, white carbon black, argil, barium sulfate or calcium carbonate; the accelerator comprises one or more of an accelerator DEU, an accelerator NA-22, an accelerator DM and an accelerator; the dispersing agent comprises fatty alcohol-polyoxyethylene ether; the anti-aging agent comprises 2-mercaptobenzimidazole or N-isopropyl-p-phenylenediamine.
The polyacrylic acids are prepared by reacting water-soluble polyether of ethylene oxide or tetrahydrofuran with isocyanate.
The preparation method of the bifunctional swelling elastomer material comprises the following steps:
1) firstly, plasticating hydrogenated nitrile rubber to obtain a hydrogenated nitrile rubber dispersoid;
2) banburying the hydrogenated nitrile rubber dispersoid and all other raw materials according to a ratio;
3) banburying and then mixing;
4) mixing and then extruding for molding;
5) pre-vulcanizing the mixed molding product to obtain a semi-finished product;
6) and performing two-stage vulcanization on the semi-finished product to obtain a finished product.
In the preparation method, the prevulcanization time in the step 5) is 20-30 minutes, the prevulcanization temperature is 140-150 ℃, and the prevulcanization pressure is 10-20 Mpa.
The second-stage vulcanization time in the step 6) is 2-3 hours, the temperature of the second-stage vulcanization is 160-180 ℃, and the pressure of the second-stage vulcanization is 10-20 Mpa.
Mixing by using an open mill in the step 3); and 4) mixing, putting into an extruder, and extruding and molding.
The prepared difunctional expandable elastomer material is characterized in that a hydrophilic oleophilic group or a hydrophilic oleophilic component is introduced into a rubber matrix, and the difunctional expandable elastomer material can expand and generate larger expansion pressure after absorbing oil and water; the oil absorption and absorption material has good water absorption and oil absorption performance, strong chemical stability, high liquid absorption expansion rate, high strength, durability and reusability; the preparation method adopts a continuous extrusion vulcanization process, has the advantages of less processing procedures, labor and raw material saving and the like, has stable product quality, high yield and high work efficiency, and is suitable for mass production; the waterproof and moisture-proof sealed packaging film can be applied to engineering facilities such as tunnels, subways, culverts, buildings, underground engineering, land or offshore oil extraction and the like, is also an ideal waterproof and moisture-proof sealed package for automobiles, containers, precise instruments, medicines, foods and the like, and has wide application prospect.
Detailed Description
The invention is further illustrated by the following examples.
In comprehensive embodiment 1, a bifunctional expandable elastomer material comprises the following raw materials in percentage by mass: 20-30 parts by mass of hydrogenated nitrile rubber; one or two of Natural Rubber (NR) and synthetic rubber (3-10 parts by mass), wherein the synthetic rubber is one or more of styrene-butadiene rubber (SBR), polyisoprene (IR), butyl rubber (IIR), polybutadiene rubber (PBR) and acrylonitrile-butadiene copolymer (NBR); the swelling component (i.e., the functional component or the liquid-absorbing polymeric material) may be optionally present in one or more of the following materialsThe modified black carbon black concrete comprises 30-35 parts by mass of modified black carbon, high-sodium bentonite, white carbon black, polyvinyl alcohol, starch grafted acrylamide-methyl methacrylate copolymer (SMAAM), maleic anhydride graft (MA), hydrophilic polyurethane Prepolymer (PU), Polyacrylic Acid (PAC), Polyacrylate (PAAS), Polyacrylamide (PAM) and acrylic acid modifier (GPAC) which are prepared by reacting water-soluble polyether of ethylene oxide or tetrahydrofuran with isocyanate; the reinforcing filler comprises one or more of black carbon black, white carbon black, argil, barium sulfate or calcium carbonate, and 8-9 parts by mass; 2-3 parts by mass of a polyether diol is preferably selected as the curing agent; the accelerant comprises one or more of accelerant DEU, accelerant NA-22, accelerant DM and accelerant, and the mass portion is 0.4-1.0; the dispersant comprises sodium stearate (C)17H35COONa), sodium dodecylbenzenesulfonate (C)18H29NaO3S), sodium lauryl sulfate (C)12H25SO4Na) or fatty alcohol-polyoxyethylene ether 2-4 parts by mass; the anti-aging agent is selected from 2-mercaptobenzimidazole or N-isopropyl p-phenylenediamine, and comprises 0.5-1.0 part by mass of anti-aging agent 4010, anti-aging agent 4020 and anti-aging agent 4040 NA; 1.0-2.5 parts by mass of zinc oxide; 0.5 to 1.0 mass part of magnesium oxide.
Wherein the polyacrylic acid is prepared by reacting water-soluble polyether of ethylene oxide or tetrahydrofuran with isocyanate.
In comprehensive embodiment 2, the preparation method of the bifunctional temperature-resistant expandable elastomer material based on the raw materials and the mixture ratio comprises the following steps:
1) plasticating: firstly, plasticating hydrogenated nitrile rubber to obtain a hydrogenated nitrile rubber dispersoid;
2) banburying: banburying the raw materials according to the proportion;
3) mixing: mixing by an open mill;
4) extruding: mixing and putting into an extruder for extrusion;
5) pre-vulcanizing: pre-vulcanizing the rubber compound to obtain a semi-finished product, wherein the pre-vulcanization time is 20-30 minutes, the pre-vulcanization temperature is 140-150 ℃, and the pre-vulcanization pressure is 10-20 Mpa;
6) secondary vulcanization: and performing secondary vulcanization on the semi-finished product, wherein the secondary vulcanization time is 2-3 hours, the temperature of the secondary vulcanization is 160-180 ℃, and the pressure of the secondary vulcanization is 10-20 Mpa, so as to obtain the finished product.
In the preparation method, the plastication leads the hydrogenated nitrile rubber to be broken from a long-chain structure into a short-chain structure, the molecular weight is reduced, and the viscosity is reduced, thereby facilitating the subsequent mixing.
During mixing, the mixing temperature and the mixing ratio of the elastomer must be controlled to ensure that the elastomer prepolymer does not self-polymerize, and the hydrogenated nitrile rubber, various elastomer prepolymers and the compounding agent after mixing are macroscopically uniformly dispersed under the action of the surfactant.
The hydrogenated nitrile rubber and various elastomers are partially chemically crosslinked, and form respective networks which are mutually penetrated under the traction of the action of a dispersing agent to form a physical interpenetrating network system (IPN). The IPN is characterized in that the two networks have synergistic effect, namely the comprehensive performance of the IPN exceeds the respective performance superposition of each component, so that the IPN has high temperature resistance, ozonization resistance, wear resistance and excellent performance and can be ensured.
Specific examples are given below for further explanation.
The formula of typical examples 1-6 of the temperature resistant material of the bifunctional swelling elastomer is given in Table 1, and the unit is part by mass. Wherein the selection of the raw materials is made according to the above-mentioned general example 1.
Figure 573666DEST_PATH_IMAGE001
With the formulation of example 4 as the starting material, plastication was first carried out: firstly, plasticating hydrogenated nitrile rubber to obtain a hydrogenated nitrile rubber dispersoid; sequentially adding the raw materials into an internal mixer, mixing for 10 minutes at 60 ℃, and taking out; mixing in an open mill, putting the mixed rubber material into an extruder, ensuring the rubber material to be sufficient in the cavity of the extruder and not to be short of the rubber material, adjusting the rotating speed of a screw and a side pressure roller, controlling the width and the thickness of the discharged rubber material, properly slowing down the extrusion speed if the width is too wide, properly accelerating the extrusion speed if the width is too narrow, setting the conveying speed of each section, controlling the conveying speed to be 5-5.5 m/min, and controlling the temperature of cooling water of each section to be below 60 ℃. Extruding: mixing and putting into an extruder for extrusion; then carrying out prevulcanization: pre-vulcanizing the rubber compound to obtain a semi-finished product, wherein the pre-vulcanization time is 20-30 minutes, the pre-vulcanization temperature is 140-150 ℃, and the pre-vulcanization pressure is 10-20 Mpa; then carrying out secondary vulcanization: and performing secondary vulcanization on the semi-finished product, wherein the secondary vulcanization time is 2-3 hours, the temperature of the secondary vulcanization is 160-180 ℃, and the pressure of the secondary vulcanization is 10-20 Mpa, so as to obtain the finished product.
The results of the physical property tests of the products prepared in examples 1 to 6 are shown in Table 2:
Figure 428489DEST_PATH_IMAGE003
the data in Table 2 show that the temperature resistance of the bifunctional expanded elastomer completely meets the national technical indexes, meets the use requirements, and has excellent performance.

Claims (7)

1.一种双功能膨胀弹性体材料，其特征在于包括：氢化丁腈橡胶20 ～30质量份；天然橡胶和/或合成橡胶3 ～ 10质量份；膨胀组分30 ～ 35质量份；补强填充剂8 ～9质量份；固化剂2 ～ 3质量份；促进剂0.4 ～ 1.0质量份；分散剂2 ～ 4质量份；防老剂0.5 ～ 1.0质量份；氧化锌1.0 ～2.5质量份；氧化镁0.5 ～ 1.0质量份；1. A bifunctional expanded elastomer material, characterized in that it comprises: 20 to 30 parts by mass of hydrogenated nitrile rubber; 3 to 10 parts by mass of natural rubber and/or synthetic rubber; 30 to 35 parts by mass of swelling components; 8-9 parts by mass of filler; 2-3 parts by mass of curing agent; 0.4-1.0 parts by mass of accelerator; 2-4 parts by mass of dispersant; 0.5-1.0 parts by mass of antioxidant; 1.0-2.5 parts by mass of zinc oxide; magnesium oxide 0.5 to 1.0 parts by mass; 所述膨胀组分为淀粉接枝丙烯酰胺-甲基丙烯酸甲酯共聚物，和选自亲水性聚氨酯预聚体、聚丙烯酸、聚丙烯酸盐或聚丙烯酰胺中的一种或者几种的混合物。The swelling component is starch grafted acrylamide-methyl methacrylate copolymer, and one or more mixtures selected from hydrophilic polyurethane prepolymer, polyacrylic acid, polyacrylate or polyacrylamide . 2. 根据权利要求1 所述双功能膨胀弹性体材料，其特征在于：氢化丁腈橡胶20 ～30质量份；天然橡胶和/或合成橡胶3 ～ 10质量份；膨胀组分30.2 ～ 32.8质量份；补强填充剂8.1 ～ 8.4质量份；固化剂2.4 ～ 3.0质量份；促进剂0.4 ～ 1.0质量份；分散剂2.8 ～3.9质量份；防老剂0.8 ～ 1.0质量份；氧化锌1.2 ～2.3质量份；氧化镁0.6 ～ 1.0质量份。2. The bifunctional intumescent elastomer material according to claim 1, characterized in that: 20-30 parts by mass of hydrogenated nitrile rubber; 3-10 parts by mass of natural rubber and/or synthetic rubber; 30.2-32.8 parts by mass of swelling component 8.1-8.4 parts by mass of reinforcing filler; 2.4-3.0 parts by mass of curing agent; 0.4-1.0 parts by mass of accelerator; 2.8-3.9 parts by mass of dispersant; 0.8-1.0 parts by mass of antioxidant; 1.2-2.3 parts by mass of zinc oxide ; 0.6 to 1.0 parts by mass of magnesium oxide. 3. 根据权利要求1或2 所述双功能膨胀弹性体材料，其特征在于：所述合成橡胶包括丁苯橡胶、聚异戊二烯橡胶、丁基橡胶、聚丁二烯橡胶、丙烯腈- 丁二烯共聚物中的一种或者几种的混合物；所述补强填充剂包括炭黑、白炭黑、陶土、硫酸钡或碳酸钙的一种或几种；所述促进剂包括促进剂DEU、促进剂NA-22、促进剂DM中的一种或几种；所述分散剂包括脂肪醇聚氧乙烯醚；所述防老剂包括2- 巯基苯并咪唑。3. The bifunctional expanded elastomer material according to claim 1 or 2, wherein the synthetic rubber comprises styrene-butadiene rubber, polyisoprene rubber, butyl rubber, polybutadiene rubber, acrylonitrile- A mixture of one or more of butadiene copolymers; the reinforcing filler includes one or more of carbon black, white carbon black, clay, barium sulfate or calcium carbonate; the accelerator includes an accelerator One or more of DEU, accelerator NA-22 and accelerator DM; the dispersing agent includes fatty alcohol polyoxyethylene ether; the antioxidant includes 2-mercaptobenzimidazole. 4. 根据权利要求3 所述的双功能膨胀弹性体材料的制备方法，其特征在于包括：4. The preparation method of bifunctional expanded elastomer material according to claim 3, is characterized in that comprising: 1）先将氢化丁腈橡胶塑炼，得到氢化丁腈橡胶分散体；1) First masticate the hydrogenated nitrile rubber to obtain a hydrogenated nitrile rubber dispersion; 2) 将氢化丁腈橡胶分散体和其它所有原料按配比进行密炼；2) Banbury the hydrogenated nitrile rubber dispersion and all other raw materials according to the proportions; 3) 密炼后混炼；3) Mixing after mixing; 4) 混炼后挤出成型；4) Extrusion molding after mixing; 5)将混炼后的成型产物进行预硫化，得到半成品；5) pre-vulcanizing the kneaded molded product to obtain a semi-finished product; 6)将所述半成品进行二段硫化，得到成品。6) The semi-finished product is subjected to two-stage vulcanization to obtain a finished product. 5. 根据权利要求4所述的双功能膨胀弹性体材料的制备方法，其特征在于：所述步骤5)预硫化时间为20 分钟～ 30 分钟，预硫化的温度为140℃～ 150℃，预硫化的压力为10MPa ～ 20MPa 。5. The method for preparing a bifunctional expanded elastomer material according to claim 4, wherein in the step 5) the pre-vulcanization time is 20 minutes to 30 minutes, the pre-vulcanization temperature is 140° C. to 150° C., The vulcanization pressure is 10MPa to 20MPa. 6.根据权利要求5所述的双功能膨胀弹性体材料的制备方法，其特征在于：所述步骤6)二段硫化时间为2 小时～ 3 小时，二段硫化的温度为160℃～ 180℃，二段硫化的压力为10MPa ～ 20MPa。6 . The method for preparing a bifunctional expanded elastomer material according to claim 5 , wherein in the step 6) the second-stage vulcanization time is 2 hours to 3 hours, and the second-stage vulcanization temperature is 160° C. to 180° C. 7 . , the pressure of the two-stage vulcanization is 10MPa ~ 20MPa. 7.根据权利要求6所述的双功能膨胀弹性体材料的制备方法，其特征在于：所述步骤3)采用开炼机混炼；步骤4) 混炼后放入挤出机内挤出成型。7. The preparation method of the bifunctional expanded elastomer material according to claim 6, characterized in that: in the step 3) kneading with an open mill; in the step 4) after kneading, put it into an extruder for extrusion molding .
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