CN105566571A - Preparation method of pre-crosslinked starch-based low-residue thickening agent - Google Patents
Preparation method of pre-crosslinked starch-based low-residue thickening agent Download PDFInfo
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- CN105566571A CN105566571A CN201610088315.5A CN201610088315A CN105566571A CN 105566571 A CN105566571 A CN 105566571A CN 201610088315 A CN201610088315 A CN 201610088315A CN 105566571 A CN105566571 A CN 105566571A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F251/00—Macromolecular compounds obtained by polymerising monomers on to polysaccharides or derivatives thereof
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B31/00—Preparation of derivatives of starch
- C08B31/18—Oxidised starch
- C08B31/185—Derivatives of oxidised starch, e.g. crosslinked oxidised starch
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K8/00—Compositions for drilling of boreholes or wells; Compositions for treating boreholes or wells, e.g. for completion or for remedial operations
- C09K8/60—Compositions for stimulating production by acting on the underground formation
- C09K8/62—Compositions for forming crevices or fractures
- C09K8/66—Compositions based on water or polar solvents
- C09K8/68—Compositions based on water or polar solvents containing organic compounds
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K8/00—Compositions for drilling of boreholes or wells; Compositions for treating boreholes or wells, e.g. for completion or for remedial operations
- C09K8/60—Compositions for stimulating production by acting on the underground formation
- C09K8/84—Compositions based on water or polar solvents
- C09K8/86—Compositions based on water or polar solvents containing organic compounds
- C09K8/88—Compositions based on water or polar solvents containing organic compounds macromolecular compounds
- C09K8/90—Compositions based on water or polar solvents containing organic compounds macromolecular compounds of natural origin, e.g. polysaccharides, cellulose
Abstract
The invention relates to a preparation method of a pre-crosslinked starch-based low-residue thickening agent, and belongs to the technical field of thickening agent preparation. The method comprises the steps that starch is mixed with ammonium persulfate, hydrogen peroxide and deionized water, ultrasonic dispersion, standing and oxidation are conducted, and oxidized starch liquid is obtained; gelatinization is conducted on the oxidized starch liquid through heating in a water bath, the pH is adjusted, and modified starch liquid is obtained; the modified starch liquid is mixed with substances such as sorbitan fatty acid ester and potassium persulfate, a reaction is conducted, and crosslinked starch modified liquid is obtained; a potassium chloride solution and a boric acid solution are added, and a starch-based thickening agent base solution is prepared; under the action of potassium persulfate, heating in the water bath, centrifugal filtration and concentration are conducted, and the thickening agent is obtained. According to the preparation method of the pre-crosslinked starch-based low-residue thickening agent, the situation that a large number of residues are generated due to the fact that crosslinking is caused is not prone to occurrence in use, and the residue rate is decreased by 10%-15%; the viscosity coefficient of the thickening agent is somewhat increased, and the viscosity coefficient at room temperature reaches 40 MPa.s or above.
Description
Technical field
The present invention relates to the preparation method of the low residue viscosifying agent of a kind of precrosslink starch base, belong to viscosifying agent preparing technical field.
Background technology
Fracturing technique is conventional yield-increasing technology, for waterfrac treatment fracturing liquid type and performance thereof and produce certain size, there is the crack of flow conductivity have close relationship, the important factor affecting pressure break success or failure, therefore to of the fracturing fluid performance as the performances such as tackifying, rheological, leak-off, friction loss, stability, formation damage all have strict requirement.Wherein, the thickening material (i.e. viscosifying agent) as raising fracturing liquid viscosity is of the fracturing fluid major ingredient.
Usually, in the process implementing fracturing yield increasing, suitable fracturing fluid system be selected, to reduce the extent of injury of fracturing liquid to reservoir and crack.At present, what domestic use was more is still plant gum fracturing fluid system, but the water-insoluble existed in this system is more, even if adopt one-level hydroxypropyl guanidine that glue, its water-insoluble is also more than 8%.Meanwhile, during use plant gum fracturing fluid system, residue is also more, and the injury in this formation and crack is larger.And the functional group that natural polymer and modified product (as various modification guanidine glue) thereof can occur to be cross-linked is many, easily there is crosslinking reaction, become the main thickening material of domestic and international fracturing liquid.But itself contain more water-insoluble (8 ~ 10%), the source of this fracturing fluid residue, except insolubles own, also has broken glue not thorough in addition.
Summary of the invention
Technical problem to be solved by this invention: easily crosslinking reaction occurs after a procedure for the natural polymer subclass thickening material used at present, containing more insolubles in water, residue is more, its broken glue is not thorough simultaneously, provide a kind of connecing on starch group and prop up an Acrylic Acid Monomer, make it in use not easily occur crosslinked and produce a large amount of residues, its viscous modulus also can increase simultaneously, and its viscosity at ambient temperature coefficient reaches more than 40MPas.
For solving the problems of the technologies described above, the present invention adopts technical scheme as described below to be:
(1) count by weight, weigh 25 ~ 40 parts of starch, 5 ~ 10 parts of ammonium persulphates, 10 ~ 15 parts of hydrogen peroxide and 45 ~ 50 parts of deionized waters respectively, at 200 ~ 300W ultrasonic disperse, 10 ~ 15min, leave standstill oxidation 1 ~ 2h, be prepared into oxidized starch solution, subsequently oxidized starch solution be placed in 65 ~ 70 DEG C of water-baths and heat, make its gelatinization 2 ~ 3h, regulate pH to 8.0 with the sodium hydroxide solution that mass concentration is 20%, prepare treated starch liquid;
(2) the treated starch liquid of above-mentioned preparation is collected, make it leave standstill and be cooled to 20 ~ 30 DEG C, count by weight subsequently, weigh 45 ~ 65 parts respectively and leave standstill cooled treated starch liquid, 2 ~ 3 parts of anhydrosorbitol acid anhydride fatty acid esters, 3 ~ 4 parts of sodium bisulfites, 5 ~ 8 parts of Potassium Persulphates and 25 ~ 40 parts of acrylate in four-hole boiling flask, be uniformly mixed and lead to nitrogen excluding air, subsequently under nitrogen protection, be placed on 68 ~ 75 DEG C of heating in water bath 2 ~ 3h, after question response completes, stop stirring, leave standstill and be cooled to 20 ~ 30 DEG C, be prepared into crosslinked starch modified liquid;
(3) 1:5 in mass ratio, be that the Klorvess Liquid of 10% and the crosslinked starch modified liquid of above-mentioned preparation are uniformly mixed by mass concentration, and be placed in beaker, dripping the mass concentration identical with Klorvess Liquid volume is subsequently 3% boric acid solution, control rate of addition is 1mL/min, after being added dropwise to complete, regulating pH to 9.5 with the sodium hydroxide solution that mass concentration is 10% again, being prepared into starch base viscosifying agent base fluid;
(4) 1:5 in mass ratio, Potassium Persulphate is added in the starch base viscosifying agent base fluid of above-mentioned preparation, be uniformly mixed and be placed in 78 ~ 80 DEG C of water-bath heating 1 ~ 2h, after broken glue completes, left standstill and be cooled to 20 ~ 30 DEG C, move in rotating speed 2500 ~ 3000r/min whizzer subsequently, centrifugation 10 ~ 15min, collect supernatant liquid and it is filtered, filtrate is placed in Rotary Evaporators, rotary evaporation, to 1/2 of original volume, can be prepared into the low residue viscosifying agent of a kind of precrosslink starch base.
The low residue viscosifying agent of precrosslink starch base prepared by the present invention its be white powder, viscosity at ambient temperature coefficient reaches more than 40MPas, and crosslinking time is 15 ~ 20s, and residue content is 30 ~ 40mg/L, and breaking glue solution surface tension is 20 ~ 25mN/m.
The present invention is compared with additive method, and Advantageous Effects is:
(1) the low residue viscosifying agent of precrosslink starch base that prepared by the present invention in use not easily occurs crosslinked and produces a large amount of residues, and residue rate reduces 10 ~ 15%;
(2) its viscous modulus also can increase, and viscosity at ambient temperature coefficient reaches more than 40MPas;
(3) preparation process of the present invention is simple, and required cost is low.
Embodiment
First count by weight, weigh 25 ~ 40 parts of starch, 5 ~ 10 parts of ammonium persulphates, 10 ~ 15 parts of hydrogen peroxide and 45 ~ 50 parts of deionized waters respectively, at 200 ~ 300W ultrasonic disperse, 10 ~ 15min, leave standstill oxidation 1 ~ 2h, be prepared into oxidized starch solution, subsequently oxidized starch solution be placed in 65 ~ 70 DEG C of water-baths and heat, make its gelatinization 2 ~ 3h, regulate pH to 8.0 with the sodium hydroxide solution that mass concentration is 20%, prepare treated starch liquid; Collect the treated starch liquid of above-mentioned preparation, make it leave standstill and be cooled to 20 ~ 30 DEG C, count by weight subsequently, weigh 45 ~ 65 parts respectively and leave standstill cooled treated starch liquid, 2 ~ 3 parts of anhydrosorbitol acid anhydride fatty acid esters, 3 ~ 4 parts of sodium bisulfites, 5 ~ 8 parts of Potassium Persulphates and 25 ~ 40 parts of acrylate in four-hole boiling flask, be uniformly mixed and lead to nitrogen excluding air, subsequently under nitrogen protection, be placed on 68 ~ 75 DEG C of heating in water bath 2 ~ 3h, after question response completes, stop stirring, leave standstill and be cooled to 20 ~ 30 DEG C, be prepared into crosslinked starch modified liquid; 1:5 in mass ratio again, be that the Klorvess Liquid of 10% and the crosslinked starch modified liquid of above-mentioned preparation are uniformly mixed by mass concentration, and be placed in beaker, dripping the mass concentration identical with Klorvess Liquid volume is subsequently 3% boric acid solution, control rate of addition is 1mL/min, after being added dropwise to complete, regulating pH to 9.5 with the sodium hydroxide solution that mass concentration is 10% again, being prepared into starch base viscosifying agent base fluid; Then 1:5 in mass ratio, Potassium Persulphate is added in the starch base viscosifying agent base fluid of above-mentioned preparation, be uniformly mixed and be placed in 78 ~ 80 DEG C of water-bath heating 1 ~ 2h, after broken glue completes, left standstill and be cooled to 20 ~ 30 DEG C, move in rotating speed 2500 ~ 3000r/min whizzer subsequently, centrifugation 10 ~ 15min, collect supernatant liquid and it is filtered, filtrate is placed in Rotary Evaporators, rotary evaporation, to 1/2 of original volume, can be prepared into the low residue viscosifying agent of a kind of precrosslink starch base.
Example 1
First count by weight, weigh 40 parts of starch, 5 parts of ammonium persulphates, 10 parts of hydrogen peroxide and 45 parts of deionized waters respectively, at 300W ultrasonic disperse 15min, leave standstill oxidation 2h, be prepared into oxidized starch solution, subsequently oxidized starch solution be placed in 70 DEG C of water-baths and heat, make its gelatinization 3h, regulate pH to 8.0 with the sodium hydroxide solution that mass concentration is 20%, prepare treated starch liquid; Collect the treated starch liquid of above-mentioned preparation, make it leave standstill and be cooled to 30 DEG C, count by weight subsequently, weigh 65 parts respectively and leave standstill cooled treated starch liquid, 2 parts of anhydrosorbitol acid anhydride fatty acid esters, 3 parts of sodium bisulfites, 5 parts of Potassium Persulphates and 25 parts of acrylate in four-hole boiling flask, be uniformly mixed and lead to nitrogen excluding air, subsequently under nitrogen protection, be placed on 75 DEG C of heating in water bath 3h, after question response completes, stop stirring, leave standstill and be cooled to 30 DEG C, be prepared into crosslinked starch modified liquid; 1:5 in mass ratio again, be that the Klorvess Liquid of 10% and the crosslinked starch modified liquid of above-mentioned preparation are uniformly mixed by mass concentration, and be placed in beaker, dripping the mass concentration identical with Klorvess Liquid volume is subsequently 3% boric acid solution, control rate of addition is 1mL/min, after being added dropwise to complete, regulating pH to 9.5 with the sodium hydroxide solution that mass concentration is 10% again, being prepared into starch base viscosifying agent base fluid; Then 1:5 in mass ratio, Potassium Persulphate is added in the starch base viscosifying agent base fluid of above-mentioned preparation, be uniformly mixed and be placed in 78 DEG C of water-baths and heat 1h, after broken glue completes, left standstill and be cooled to 30 DEG C, move in rotating speed 2500r/min whizzer subsequently, centrifugation 15min, collects supernatant liquid and filters it, filtrate is placed in Rotary Evaporators, rotary evaporation, to 1/2 of original volume, can be prepared into the low residue viscosifying agent of a kind of precrosslink starch base.The low residue viscosifying agent of precrosslink starch base prepared by the present invention in use not easily occurs crosslinked and produces a large amount of residues, and residue rate reduces 15%, and its viscous modulus also can increase, and viscosity at ambient temperature coefficient reaches 41MPas; Preparation process is simple, and required cost is low.
Example 2
First count by weight, weigh 25 parts of starch, 10 parts of ammonium persulphates, 15 parts of hydrogen peroxide and 50 parts of deionized waters respectively, at 200W ultrasonic disperse 10min, leave standstill oxidation 1h, be prepared into oxidized starch solution, subsequently oxidized starch solution be placed in 65 DEG C of water-baths and heat, make its gelatinization 2h, regulate pH to 8.0 with the sodium hydroxide solution that mass concentration is 20%, prepare treated starch liquid; Collect the treated starch liquid of above-mentioned preparation, make it leave standstill and be cooled to 20 DEG C, count by weight subsequently, weigh 45 parts respectively and leave standstill cooled treated starch liquid, 3 parts of anhydrosorbitol acid anhydride fatty acid esters, 4 parts of sodium bisulfites, 8 parts of Potassium Persulphates and 40 parts of acrylate in four-hole boiling flask, be uniformly mixed and lead to nitrogen excluding air, subsequently under nitrogen protection, be placed on 68 DEG C of heating in water bath 2h, after question response completes, stop stirring, leave standstill and be cooled to 20 DEG C, be prepared into crosslinked starch modified liquid; 1:5 in mass ratio again, be that the Klorvess Liquid of 10% and the crosslinked starch modified liquid of above-mentioned preparation are uniformly mixed by mass concentration, and be placed in beaker, dripping the mass concentration identical with Klorvess Liquid volume is subsequently 3% boric acid solution, control rate of addition is 1mL/min, after being added dropwise to complete, regulating pH to 9.5 with the sodium hydroxide solution that mass concentration is 10% again, being prepared into starch base viscosifying agent base fluid; Then 1:5 in mass ratio, Potassium Persulphate is added in the starch base viscosifying agent base fluid of above-mentioned preparation, be uniformly mixed and be placed in 78 DEG C of water-baths and heat 1h, after broken glue completes, left standstill and be cooled to 20 DEG C, move in rotating speed 2500r/min whizzer subsequently, centrifugation 10min, collects supernatant liquid and filters it, filtrate is placed in Rotary Evaporators, rotary evaporation, to 1/2 of original volume, can be prepared into the low residue viscosifying agent of a kind of precrosslink starch base.The low residue viscosifying agent of precrosslink starch base prepared by the present invention in use not easily occurs crosslinked and produces a large amount of residues, and residue rate reduces 12%, and its viscous modulus also can increase, and viscosity at ambient temperature coefficient reaches 42MPas; Preparation process is simple, and required cost is low.
Example 3
First count by weight, weigh 30 parts of starch, 10 parts of ammonium persulphates, 10 parts of hydrogen peroxide and 50 parts of deionized waters respectively, at 250W ultrasonic disperse 12min, leave standstill oxidation 1h, be prepared into oxidized starch solution, subsequently oxidized starch solution be placed in 68 DEG C of water-baths and heat, make its gelatinization 2h, regulate pH to 8.0 with the sodium hydroxide solution that mass concentration is 20%, prepare treated starch liquid; Collect the treated starch liquid of above-mentioned preparation, make it leave standstill and be cooled to 25 DEG C, count by weight subsequently, weigh 50 parts respectively and leave standstill cooled treated starch liquid, 2 parts of anhydrosorbitol acid anhydride fatty acid esters, 3 parts of sodium bisulfites, 5 parts of Potassium Persulphates and 40 parts of acrylate in four-hole boiling flask, be uniformly mixed and lead to nitrogen excluding air, subsequently under nitrogen protection, be placed on 70 DEG C of heating in water bath 2h, after question response completes, stop stirring, leave standstill and be cooled to 25 DEG C, be prepared into crosslinked starch modified liquid; 1:5 in mass ratio again, be that the Klorvess Liquid of 10% and the crosslinked starch modified liquid of above-mentioned preparation are uniformly mixed by mass concentration, and be placed in beaker, dripping the mass concentration identical with Klorvess Liquid volume is subsequently 3% boric acid solution, control rate of addition is 1mL/min, after being added dropwise to complete, regulating pH to 9.5 with the sodium hydroxide solution that mass concentration is 10% again, being prepared into starch base viscosifying agent base fluid; Then 1:5 in mass ratio, Potassium Persulphate is added in the starch base viscosifying agent base fluid of above-mentioned preparation, be uniformly mixed and be placed in 79 DEG C of water-baths and heat 1h, after broken glue completes, left standstill and be cooled to 25 DEG C, move in rotating speed 2700r/min whizzer subsequently, centrifugation 12min, collects supernatant liquid and filters it, filtrate is placed in Rotary Evaporators, rotary evaporation, to 1/2 of original volume, can be prepared into the low residue viscosifying agent of a kind of precrosslink starch base.
The low residue viscosifying agent of precrosslink starch base prepared by the present invention in use not easily occurs crosslinked and produces a large amount of residues, and residue rate reduces 10%, and its viscous modulus also can increase, and viscosity at ambient temperature coefficient reaches 45MPas; Preparation process is simple, and required cost is low.
Claims (1)
1. a preparation method for the low residue viscosifying agent of precrosslink starch base, is characterized in that concrete preparation process is:
(1) count by weight, weigh 25 ~ 40 parts of starch, 5 ~ 10 parts of ammonium persulphates, 10 ~ 15 parts of hydrogen peroxide and 45 ~ 50 parts of deionized waters respectively, at 200 ~ 300W ultrasonic disperse, 10 ~ 15min, leave standstill oxidation 1 ~ 2h, be prepared into oxidized starch solution, subsequently oxidized starch solution be placed in 65 ~ 70 DEG C of water-baths and heat, make its gelatinization 2 ~ 3h, regulate pH to 8.0 with the sodium hydroxide solution that mass concentration is 20%, prepare treated starch liquid;
(2) the treated starch liquid of above-mentioned preparation is collected, make it leave standstill and be cooled to 20 ~ 30 DEG C, count by weight subsequently, weigh 45 ~ 65 parts respectively and leave standstill cooled treated starch liquid, 2 ~ 3 parts of anhydrosorbitol acid anhydride fatty acid esters, 3 ~ 4 parts of sodium bisulfites, 5 ~ 8 parts of Potassium Persulphates and 25 ~ 40 parts of acrylate in four-hole boiling flask, be uniformly mixed and lead to nitrogen excluding air, subsequently under nitrogen protection, be placed on 68 ~ 75 DEG C of heating in water bath 2 ~ 3h, after question response completes, stop stirring, leave standstill and be cooled to 20 ~ 30 DEG C, be prepared into crosslinked starch modified liquid;
(3) 1:5 in mass ratio, be that the Klorvess Liquid of 10% and the crosslinked starch modified liquid of above-mentioned preparation are uniformly mixed by mass concentration, and be placed in beaker, dripping the mass concentration identical with Klorvess Liquid volume is subsequently 3% boric acid solution, control rate of addition is 1mL/min, after being added dropwise to complete, regulating pH to 9.5 with the sodium hydroxide solution that mass concentration is 10% again, being prepared into starch base viscosifying agent base fluid;
(4) 1:5 in mass ratio, Potassium Persulphate is added in the starch base viscosifying agent base fluid of above-mentioned preparation, be uniformly mixed and be placed in 78 ~ 80 DEG C of water-bath heating 1 ~ 2h, after broken glue completes, left standstill and be cooled to 20 ~ 30 DEG C, move in rotating speed 2500 ~ 3000r/min whizzer subsequently, centrifugation 10 ~ 15min, collect supernatant liquid and it is filtered, filtrate is placed in Rotary Evaporators, rotary evaporation, to 1/2 of original volume, can be prepared into the low residue viscosifying agent of a kind of precrosslink starch base.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107033865A (en) * | 2017-05-14 | 2017-08-11 | 常州蓝森环保设备有限公司 | A kind of preparation method of oil well wax-proofing agent |
| CN109400729A (en) * | 2018-12-03 | 2019-03-01 | 寿光金远东变性淀粉有限公司 | A method of oxidized starch is prepared using composite oxidant |
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2016
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107033865A (en) * | 2017-05-14 | 2017-08-11 | 常州蓝森环保设备有限公司 | A kind of preparation method of oil well wax-proofing agent |
| CN109400729A (en) * | 2018-12-03 | 2019-03-01 | 寿光金远东变性淀粉有限公司 | A method of oxidized starch is prepared using composite oxidant |
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Application publication date: 20160511 |