CN103848935A - Oil-absorptive resin and oil-absorptive expanding rubber comprising same - Google Patents
Oil-absorptive resin and oil-absorptive expanding rubber comprising same Download PDFInfo
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- CN103848935A CN103848935A CN201410061784.9A CN201410061784A CN103848935A CN 103848935 A CN103848935 A CN 103848935A CN 201410061784 A CN201410061784 A CN 201410061784A CN 103848935 A CN103848935 A CN 103848935A
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Abstract
The invention provides oil-absorptive resin and oil-absorptive expanding rubber comprising the same. The oil-absorptive resin comprises the following components in parts by weight: 60 to 75 parts of polymer monomer, 0.5 to 2.5 parts of catalyst, 0.5 to 1 part of initiator, 0.01 to 0.03 part of cross-linking agent and 25 to 30 parts of dispersing phase. The invention also provides expanding rubber comprising the oil-absorptive resin. The oil-absorptive expanding rubber comprises the following components in parts by weight: 100 parts of rubber, 40 to 100 parts of oil-absorptive resin, 40 to 80 parts of reinforcing agent, 10 to 20 parts of softening agent, 0.5 to 2 parts of vulcanizing agent, 0.5 to 2 parts of promoter, 0.5 to 2 parts of anti-aging agent and 6 to 8 parts of active agent. By utilizing the characteristic of the oil-absorptive resin that the oleophylic group (ester group) is interactively affine to oil molecules to absorb the oil, the prepared oil-absorptive resin has porosity, so that the expanding rubber utilizing the oil-absorptive resin has better oil-absorptive effect in comparison with the traditional oil-absorptive expanding rubber, and the pressure resisting effect is also improved.
Description
Technical field
The oil suction expanded rubber that the present invention relates to a kind of oil-absorbing resin and comprise this oil-absorbing resin, belongs to industrial expanded rubber field.
Background technology
In prior art, due to the environment harshness under oil well, common oil suction expanded rubber does not usually reach job requirements, and therefore research can be born multiduty meticulous type, functional type and the structure-type oil suction expanded rubber of environment and special occasions for a long time, is a direction of oil suction expanded rubber development.
Oil suction expanded rubber (oil swellable rubber is called for short OSR) is a kind of novel functional type oil suction elastomeric material, on traditional rubber matrix, introduce lipophilicity functional group by chemical process or make with lipophilic ingredients blend, it is the combination of rubber matrix and nonpolar lipophilic ingredient.Oil suction expanded rubber had both kept good snappiness and the compression deformability of rubber, after also having oil suction, volume expands rapidly simultaneously, under certain pressure, having stable guarantor's oiliness energy, is current optimal leak-stopping sealing material, can be widely used in multiple industry.Whether OSR has a variety of sorting techniques, vulcanize according to goods, can be divided into sulfide type (goods type) and non-vulcanization type (putty type), can be divided into physical blending type and chemical graft type by preparation method.
Oil suction expanded rubber and non-polar material surface (pitch, plastics, rubber) and polar material surface (sand-cement slurry, reinforced concrete) all have the closely sealed performance of good infiltration, can repeatedly absorb oil fast and expand, and under certain pressure, having stable guarantor's oiliness energy, is current optimal grease proofing leak-stopping sealing material.What report was maximum at present is oil suction expanded rubber to be used as to oil well meet oily swell packers, assist, strengthen the packing of traditional cement mantle to stratum or directly replace cement mantle to carry out packing to the annular space between sleeve pipe and stratum, realizing resilient seal and oil suction and expand and stop oily dual nature.Oil suction expanded rubber is applied in uncased hole or cased well, can effectively realizes the separation to different pay sands.The existing ripe product of state's affair oil swell packers at present, and put on market, mainly " cementing quality guarantee instrument " (Cement Assurance Tool) of Harry C Compaq and the ZIP(Zonal Inf low Profiler of SWELLFIX company, payzone inflow profile).
It is domestic that meet the earliest the research of oily expanding material is Wang Qiang, the Cao Aili of Institutes Of Technology Of Tianjin, they make the high oil-absorbing resin (HOAR) that has synthesized multi-component copolymer by oneself, its oil suction multiplying power is more than 30g/g, using this resinoid as properties-correcting agent, prepare oil swellable rubber (OSR), detected and proved that OSR is keeping, under enough mechanical strength, organic solvent being had to good absorptivity and self stability, below 0.6MPa time, the leak-stopping time is at 4min-17min.But, because its ultimate compression strength is lower, for the situation that is applied to horizontal well and carries out the measures such as pressure break, acidifying, still can not reach requirement, therefore, need to research and develop a kind of novel oil suction expanded rubber.
Summary of the invention
For solving the problems of the technologies described above, the oil suction expanded rubber that the object of the invention is to propose a kind of oil-absorbing resin and comprise this oil-absorbing resin, this expanded rubber can be in the time meeting better oil suction expansion character, also has stronger mechanics mechanical property.
Object of the present invention is achieved by the following technical programs:
A kind of oil-absorbing resin, by weight, this oil-absorbing resin comprises following component:
Polymer monomer 60-85 part (preferably 60-75 part), catalyzer 0.5-2.5 part, initiator 0.5-1 part, linking agent 0.01-0.03 part, disperse phase 25-30 part;
Described polymer monomer comprises butyl methacrylate, and described polymer monomer also comprises one or more the combination in ethyl acrylate, methacrylic dodecyl gallate, Propenoic acid, 2-methyl, isobutyl ester and β-dimethyl-aminoethylmethacrylate;
Described catalyzer comprises di-alcohol and/or trolamine;
Described initiator comprises benzoyl peroxide;
Described linking agent comprises diacrylate-BDO ester and/or diacrylate-1, the own diester of 6-;
Described disperse phase comprises water.
In above-mentioned oil-absorbing resin, preferred, by weight, the content of described butyl methacrylate is 40-60 part.
In above-mentioned oil-absorbing resin, preferred, by weight, the content of the combination of one or more in polymer monomer in methacrylic dodecyl gallate, Propenoic acid, 2-methyl, isobutyl ester and β-dimethyl-aminoethylmethacrylate is 15-25 part.
In above-mentioned oil-absorbing resin, in the combination of polymer monomer, the ratio of monomer can have different ratios according to the difference of the performance requirement of oil-absorbing resin.
The present invention also provides a kind of preparation method of above-mentioned oil-absorbing resin, comprises the steps:
Step 1, joins polymer monomer in reactor, stirs, and obtains mixed solution;
Step 2 adds catalyzer, linking agent, initiator (preferably in batches adding) in mixed solution, adds disperse phase to stir, and obtains reaction solution;
Step 3, by the discharging after 20 minutes-40 minutes of described reaction solution uniform stirring, leaves standstill 2h-3h, obtains described oil-absorbing resin.
Above-mentioned oil-absorbing resin is that the inside that obtained by polymerization has the particle that aperture, profile be puffy and forms.
In the preparation method of above-mentioned oil-absorbing resin, preferred, in step 1, the temperature in reactor is 10-25 DEG C.
The present invention also provides a kind of oil suction expanded rubber that comprises above-mentioned oil-absorbing resin, and by weight, this oil suction expanded rubber comprises following component:
100 parts of rubber, oil-absorbing resin 40-100 part, strengthening agent 40-80 part, tenderizer 10-20 part, vulcanizing agent 0.5-2 part, promotor 0.5-2 part, anti-aging agent 0.5-2 part, promoting agent 6-8 part;
Described rubber comprises one or more the combination in paracril, chloroprene rubber, natural rubber and ethylene-propylene rubber(EPR);
Described strengthening agent comprises white carbon black and/or carbon black;
Described tenderizer comprises one or more the combination in stearic acid, naphthenic oil, dibutyl phthalate and dioctyl phthalate (DOP);
Described vulcanizing agent comprises one or more the combination in sulphur, dicumyl peroxide base resol, halogenated alkyl resol, p-benzoqui(o)none dioxime and dibenzoyl paraquinonedioxime;
Described promotor comprises one or more the combination in 2,2'-dithio-bis-benzothiazole, tetramethyl-thiuram disulfide and N-cyclohexyl-2-benzothiazole sulfonamide;
Described anti-aging agent comprises N cyclohexyl N' phenyl P phenylene diamine and/or N-sec.-propyl-N'-diphenyl-para-phenylene diamine;
Described promoting agent comprises zinc oxide and/or magnesium oxide.
The present invention also provides the preparation method of the above-mentioned oil suction expanded rubber that comprises oil-absorbing resin, comprises the steps:
Step 1 is carried out banburying by rubber and oil-absorbing resin in Banbury mixer, obtains banburying crude product;
Then step 2, mixingly in mill evenly descend that sheet is cooling to be parked to adding in banburying crude product after vulcanizing agent, strengthening agent, promoting agent, tenderizer, promotor and anti-aging agent (preferably adding successively), obtains out refining crude product;
Step 3, treat the storage period finish after according to the required weight of mould split refining crude product carry out cutting, in vulcanizing press, vulcanize, obtain described oil suction expanded rubber.
In the preparation method of the above-mentioned oil suction expanded rubber that comprises oil-absorbing resin, preferably, in step 1, banburying parameter is: banburying temperature is controlled at 120-130 DEG C, spinner velocity control is 50-80r/min, ram piston pressure is 0.2-0.6MPa, dump temperature is 90 DEG C, and the time of banburying is 20min-30min.Described Banbury mixer is the GK400 type that Dalian Hua Han Banbury mixer factory produces.
In the preparation method of the above-mentioned oil suction expanded rubber that comprises oil-absorbing resin, preferred, in step 2, mill mixing parameter is: mill mixer roller temperature is controlled at below 40 DEG C, and roller speed is 1100-1500 rev/min, and lower cooling time of parking will be 24h.
The present invention also provides the application as down-hole sealing material of above-mentioned oil suction expanded rubber, described application is the in the situation that of carrying out the measures such as pressure break, acidifying at horizontal well, oil suction expanded rubber is used as to oil well and meets oily swell packers, assist, strengthen the packing of traditional cement mantle to stratum or directly replace cement mantle to carry out packing to the annular space between sleeve pipe and stratum, realizing resilient seal and oil suction and expand and stop oily dual nature; Or oil suction expanded rubber is applied in uncased hole or cased well, realizes the separation to different pay sands.
Outstanding effect of the present invention is:
The characteristic of oil suction is prepared oil-absorbing resin with the mutual affinity interaction of oil molecule to utilize oil-absorbing resin lipophilic group (ester group), and the oil-absorbing resin making has porousness, speed of oil absorption is fast especially, uses the oil suction expanded rubber of this oil-absorbing resin to have the following advantages compared with existing oil suction expanded rubber:
1. the expansion multiplying power of this oil suction expanded rubber is high, and the rate of expansion in diesel oil is 1000%-1800%, and the rate of expansion in crude oil is 800%-1000%, and the rate of expansion in benzene is 1200%-1880%;
2. this oil suction expanded rubber has good oil absorptiveness, and separate out without any material in expansion process, expansion process is not repeatedly, rate of expansion is controlled, mechanical property excellence after expansion, at higher temperature and pressure, its performance is still stablized as before, has enriched the applied environment of oil suction expanded rubber;
3. the preparation method of this oil suction expanded rubber is simply controlled, easy handling, raw-material low price and easily producing voluntarily, Application Areas is more extensive, the rubber production factory that is applicable to various scales applies, and is a larger expansion at present domestic and international oil field with down-hole sealing material.
Embodiment
Below by specific embodiment, the present invention is described in further detail, so that technical solution of the present invention is easier to understand, grasp.
Embodiment 1
The present embodiment provides a kind of oil-absorbing resin, and by weight, this oil-absorbing resin comprises following component:
50 parts of butyl methacrylate, 20 parts of methacrylic dodecyl gallates, 1.5 parts of di-alcohol, 1 part of benzoyl peroxide (BPO), 0.01 part of diacrylate-BDO ester, 30 parts, water.
Above-mentioned oil-absorbing resin prepares by following method:
Step 1 by butyl methacrylate, methacrylic dodecyl gallate, joins in reactor under the temperature condition of 25 DEG C, stirs, and obtains mixed solution;
Step 2 adds di-alcohol, benzoyl peroxide (BPO), diacrylate-BDO ester in mixed solution in batches, and adding water is that disperse phase disperses, and stirs, and obtains reaction solution;
Step 3, by the discharging after 30 minutes of reaction solution uniform stirring, 3h post polymerization becomes inside and has the particle that aperture, profile are puffy, obtains oil-absorbing resin.
The oil-absorbing resin of gained is carried out to oil suction test, and its method is as follows:
Take 1g oil-absorbing resin and put in oily medium to be measured, after resin is fully swelling, be filtered to oil with the mesh bag that mesh chi is 0.180mm and drain, measure and drain quality, calculate and obtain oil-absorbing resin oil suction multiplying power in this testing liquid by formula below.
Formula: Q=(m
2-m
1)/m
0, wherein: m
0for the quality before resin oil suction, m
1the quality of the oily medium going out for drop, m
2for the quality of oily medium to be measured.
The oil suction multiplying power (oil suction multiplying power refers to the amount of 1g liquid that absorption agent absorbs) of oil-absorbing resin is as shown in table 1:
Table 1
| Sequence number | Soak medium | Oil suction multiplying power (%) |
| 1 | Diesel oil | 1788 |
| 2 | Crude oil | 954 |
| 3 | Benzene | 1560 |
Embodiment 2
The present embodiment provides a kind of oil-absorbing resin, and by weight, this oil-absorbing resin comprises following component:
60 parts of butyl methacrylate, 10 parts of ethyl acrylates, 15 parts of Propenoic acid, 2-methyl, isobutyl esters, 1.5 parts of di-alcohol, 1 part of benzoyl peroxide (BPO), 0.01 part of diacrylate-BDO ester, 30 parts, water.
Above-mentioned oil-absorbing resin prepares by following method:
Step 1 by butyl methacrylate, ethyl acrylate, Propenoic acid, 2-methyl, isobutyl ester, joins in reactor under the temperature condition of 25 DEG C, stirs, and obtains mixed solution;
Step 2 adds di-alcohol, benzoyl peroxide (BPO), diacrylate-BDO ester in mixed solution in batches, and adding water is that disperse phase disperses, and stirs, and obtains reaction solution;
Step 3, by the discharging after 20 minutes of reaction solution uniform stirring, 2h post polymerization becomes inside and has the particle that aperture, profile are puffy, obtains oil-absorbing resin.
The oil-absorbing resin of gained is carried out to oil suction test, and its method is as follows:
Take 1g oil-absorbing resin and put in oily medium to be measured, after resin is fully swelling, be filtered to oil with the mesh bag that mesh chi is 0.180mm and drain, measure and drain quality, calculate and obtain oil-absorbing resin oil suction multiplying power in this testing liquid by formula below.
Formula: Q=(m
2-m
1)/m
0, wherein: m
0for the quality before resin oil suction, m
1the quality of the oily medium going out for drop, m
2for the quality of oily medium to be measured.
The oil suction multiplying power of oil-absorbing resin is as shown in table 2:
Table 2
| Sequence number | Soak medium | Oil suction multiplying power (%) |
| 1 | Diesel oil | 1650 |
| 2 | Crude oil | 890 |
| 3 | Benzene | 1390 |
Embodiment 3
The present embodiment provides the oil suction expanded rubber of the oil-absorbing resin of a kind of embodiment of comprising 1, and by weight, this oil suction expanded rubber comprises following component:
1 part of 100 parts of paracril, 80 parts of oil-absorbing resins, 60 parts of carbon blacks, 2 parts of stearic acid, 0.5 part, sulphur, 10 parts of dibutyl phthalates (DBP), tetramethyl-thiuram disulfide (TMTD), 2,0.5 part of 2'-dithio-bis-benzothiazole (DM), 1 part of N-sec.-propyl-N'-phenyl-p-phenylenediamine (4010NA), 8 parts, zinc oxide.
Above-mentioned oil suction expanded rubber is prepared according to following steps:
Step 1, oil-absorbing resin prepared by paracril and embodiment 1 carries out banburying in Banbury mixer, Banbury mixer is GK400 type, banburying temperature is controlled at 120-130 DEG C, spinner velocity control is 50r/min, and ram piston pressure is 0.3MPa, and dump temperature is 90 DEG C, banburying discharging after 20 minutes, obtains banburying crude product;
Step 2, banburying crude product is moved into mill, put into successively carbon black, stearic acid, sulphur, dibutyl phthalate (DBP), tetramethyl-thiuram disulfide (TMTD), 2, after 2'-dithio-bis-benzothiazole (DM), N-sec.-propyl-N'-phenyl-p-phenylenediamine (4010NA), zinc oxide, in mill, carry out mixing, mill mixer roller temperature is controlled at below 40 DEG C, and roller speed is 1200 revs/min, mixing evenly rear lower sheet, the cooling 24h that parks, obtains out refining crude product;
Step 3, treat the storage period finish after according to the required weight of mould split refining crude product carry out cutting, in vulcanizing press, vulcanize, obtain this oil suction expanded rubber.
Oil suction expanded rubber to gained is tested: wherein, the examination criteria of tensile strength and tensile yield is as the criterion with GB/T528-2009, and hardness test standard is as the criterion with GB/T531.1-2008.
The performance of the oil suction expanded rubber of gained is as shown in table 3:
Table 3
Embodiment 4
The present embodiment provides the oil suction expanded rubber of the oil-absorbing resin of a kind of embodiment of comprising 2, and by weight, this oil suction expanded rubber comprises following component:
1 part of 100 parts of paracril, 80 parts of oil-absorbing resins, 50 parts of carbon blacks, 2 parts of stearic acid, 0.5 part, sulphur, 10 parts of dioctyl phthalate (DOP)s (DOP), N-cyclohexyl-2-benzothiazole sulfonamide (CZ), 2,0.5 part of 2'-dithio-bis-benzothiazole (DM), (4010) 1 parts of N cyclohexyl N' phenyl P phenylene diamines, 8 parts, zinc oxide.
Above-mentioned oil suction expanded rubber is prepared as follows:
Step 1, oil-absorbing resin prepared by paracril and embodiment 2 carries out banburying in Banbury mixer, Banbury mixer is GK400 type, banburying temperature is controlled at 120-130 DEG C, spinner velocity control is 50r/min, and ram piston pressure is 0.3MPa, and dump temperature is 90 DEG C, banburying discharging after 20 minutes, obtains banburying crude product;
Step 2, banburying crude product is moved into mill, put into successively zinc oxide, stearic acid, carbon black, dioctyl phthalate (DOP) (DOP), N-cyclohexyl-2-benzothiazole sulfonamide (CZ), 2, after 2'-dithio-bis-benzothiazole (DM), sulphur, N cyclohexyl N' phenyl P phenylene diamine (4010), in mill, carry out mixing, mill mixer roller temperature is controlled at below 40 DEG C, and roller speed is 1200 revs/min, mixing evenly rear lower sheet, the cooling 24h that parks, obtains out refining crude product;
Step 3, treat the storage period finish after according to the required weight of mould split refining crude product carry out cutting, in vulcanizing press, vulcanize and obtain this oil suction expanded rubber.
Oil suction expanded rubber to gained is tested:
Wherein, the examination criteria of tensile strength and tensile yield is as the criterion with GB/T528-2009, and hardness test standard is as the criterion with GB/T531.1-2008.
The performance of the oil suction expanded rubber of gained is as shown in table 4:
Table 4
From the above embodiments, the oil suction expanded rubber of being prepared by oil-absorbing resin of the present invention has excellent mechanical property before expansion, and after expansion, still has considerable mechanics mechanical property; Oil suction rate of expansion is high, has higher market application foreground.
Claims (10)
1. an oil-absorbing resin, by weight, this oil-absorbing resin comprises following component:
Polymer monomer 60-85 part, catalyzer 0.5-2.5 part, initiator 0.5-1 part, linking agent 0.01-0.03 part, disperse phase 25-30 part;
Described polymer monomer comprises butyl methacrylate, and described polymer monomer also comprises one or more the combination in ethyl acrylate, methacrylic dodecyl gallate, Propenoic acid, 2-methyl, isobutyl ester and β-dimethyl-aminoethylmethacrylate;
Described catalyzer comprises di-alcohol and/or trolamine;
Described initiator comprises benzoyl peroxide;
Described linking agent comprises diacrylate-BDO ester and/or diacrylate-1, the own diester of 6-;
Described disperse phase comprises water.
2. oil-absorbing resin according to claim 1, is characterized in that: by weight, the content of described butyl methacrylate is 40-60 part.
3. oil-absorbing resin according to claim 2, is characterized in that: by weight, the content of the combination of one or more in polymer monomer in methacrylic dodecyl gallate, Propenoic acid, 2-methyl, isobutyl ester and β-dimethyl-aminoethylmethacrylate is 15-25 part.
4. according to the preparation method of the oil-absorbing resin described in claim 1-3 any one, comprise the steps:
Step 1, joins polymer monomer in reactor, stirs, and obtains mixed solution;
Step 2 adds catalyzer, linking agent, initiator in mixed solution, adds disperse phase to stir, and obtains reaction solution;
Step 3, by the discharging after 20 minutes-40 minutes of described reaction solution uniform stirring, leaves standstill 2h-3h, obtains described oil-absorbing resin.
5. the preparation method of oil-absorbing resin according to claim 4, is characterized in that: in step 1, the temperature in reactor is 10 DEG C-25 DEG C.
6. an oil suction expanded rubber that comprises the oil-absorbing resin described in claim 1-3 any one, by weight, this oil suction expanded rubber comprises following component:
100 parts of rubber, oil-absorbing resin 40-100 part, strengthening agent 40-80 part, tenderizer 10-20 part, vulcanizing agent 0.5-2 part, promotor 0.5-2 part, anti-aging agent 0.5-2 part, promoting agent 6-8 part;
Described rubber comprises one or more the combination in paracril, chloroprene rubber, natural rubber and ethylene-propylene rubber(EPR);
Described strengthening agent comprises white carbon black and/or carbon black;
Described tenderizer comprises one or more the combination in stearic acid, naphthenic oil, dibutyl phthalate and dioctyl phthalate (DOP);
Described vulcanizing agent comprises one or more the combination in sulphur, dicumyl peroxide base resol, halogenated alkyl resol, p-benzoqui(o)none dioxime and dibenzoyl paraquinonedioxime;
Described promotor comprises one or more the combination in 2,2'-dithio-bis-benzothiazole, tetramethyl-thiuram disulfide and N-cyclohexyl-2-benzothiazole sulfonamide;
Described anti-aging agent comprises N cyclohexyl N' phenyl P phenylene diamine and/or N-sec.-propyl-N'-diphenyl-para-phenylene diamine;
Described promoting agent comprises zinc oxide and/or magnesium oxide.
7. the preparation method of the oil suction expanded rubber that comprises oil-absorbing resin claimed in claim 6, comprises the steps:
Step 1 is carried out banburying by rubber and oil-absorbing resin in Banbury mixer, obtains banburying crude product;
Step 2 adds after vulcanizing agent, strengthening agent, promoting agent, tenderizer, promotor and anti-aging agent in banburying crude product, mixingly in mill evenly then descends that sheet is cooling to be parked, and obtains out refining crude product;
Step 3, treat the storage period finish after according to the required weight of mould split refining crude product carry out cutting, in vulcanizing press, vulcanize, obtain described oil suction expanded rubber.
8. preparation method according to claim 7, is characterized in that: in step 1, banburying temperature is controlled at 120-130 DEG C, and spinner velocity is 50-80r/min, and ram piston pressure is 0.2-0.6MPa, and dump temperature is 90 DEG C, and the time of banburying is 20min-30min.
9. preparation method according to claim 7, is characterized in that, in step 2, carrying out when mixing, the bowl temperature control of mill is below 40 DEG C, and roller speed is at 1100-1500 rev/min, and lower cooling time of parking will be 24h.
10. oil suction expanded rubber claimed in claim 6 is as the application of down-hole sealing material.
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| CN108707288A (en) * | 2018-06-05 | 2018-10-26 | 汪逸凡 | A kind of oil suction rubber |
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| CN111117581B (en) * | 2019-12-30 | 2022-06-03 | 中国石油天然气股份有限公司 | Long-acting sealing agent for plugging high-angle cracks and preparation method |
| CN111454701A (en) * | 2020-02-26 | 2020-07-28 | 四川泓华油气田工程科技有限公司 | Oil-based drilling fluid expansion plugging agent |
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| CN112280194A (en) * | 2020-09-14 | 2021-01-29 | 浙江双箭橡胶股份有限公司 | Rubber material capable of expanding in presence of air and preparation method thereof |
| CN116041880A (en) * | 2023-03-20 | 2023-05-02 | 成都俊马密封科技股份有限公司 | Swelling type high-sealing gasket material and preparation method thereof |
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