CN108164606A - A kind of preparation method of drilling fluid amphoteric cellulose ether - Google Patents
A kind of preparation method of drilling fluid amphoteric cellulose ether Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B11/00—Preparation of cellulose ethers
- C08B11/02—Alkyl or cycloalkyl ethers
- C08B11/04—Alkyl or cycloalkyl ethers with substituted hydrocarbon radicals
- C08B11/14—Alkyl or cycloalkyl ethers with substituted hydrocarbon radicals with nitrogen-containing groups
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B11/00—Preparation of cellulose ethers
- C08B11/02—Alkyl or cycloalkyl ethers
- C08B11/04—Alkyl or cycloalkyl ethers with substituted hydrocarbon radicals
- C08B11/08—Alkyl or cycloalkyl ethers with substituted hydrocarbon radicals with hydroxylated hydrocarbon radicals; Esters, ethers, or acetals thereof
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- 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
- C09K8/02—Well-drilling compositions
- C09K8/03—Specific additives for general use in well-drilling compositions
- C09K8/035—Organic additives
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Abstract
The invention discloses a kind of drilling fluid preparation methods of amphoteric cellulose ether, belong to cellulose ether preparing technical field.The present invention is first under alkaline condition, etherification reaction occurs using the active hydroxyl groups on hydroxyethyl cellulose strand and epoxychloropropane and obtains cationic hydroxyethyl cellulose ethers, it is 3 chlorine, 2 hydroxypropyl dimethylammonium guanidine-acetic acid salt that thick filtrate is prepared again, improve the resistance of motion of hydrone so that cellulose ether has the function of splendid drop dehydration in drilling fluid；The number of anions and canons group is roughly equal in the amphoteric cellulose ether of the present invention, electrostatic force is only electrostatic attraction in its strand, polymer molecule is caused to shrink, hydrodynamic volume reduces, and solution viscosity becomes smaller, so as to show apparent anti-polyelectrolyte solution behavior, make that larger consistency still can be kept when water content is higher in drilling fluid, weaken the osmosis of salting liquid, so as to improve salt tolerance of the amphoteric cellulose ether in drilling fluid, have a extensive future.
Description
Technical field
The invention discloses a kind of drilling fluid preparation methods of amphoteric cellulose ether, belong to cellulose ether technology of preparing neck
Domain.
Background technology
Cellulose ether has the high-molecular compound of ether structure made of cellulose.Each grape in cellulose macromolecule
Glycosyl ring contains there are three hydroxyl, the primary hydroxyl on the 6th carbon atom, the secondary hydroxyl on second and third carbon atom, the hydrogen in hydroxyl
Replaced by alkyl and generate cellulose ether derivatives.It is the product that the hydrogen of hydroxyl in cellulosic polymer is replaced by alkyl.
Cellulose is a kind of polyhydroxy high-molecular compound for both not dissolved or not melted.Water, dilute can be then dissolved in after cellulose is etherified
Aqueous slkali and organic solvent, and with thermoplasticity.
According to the classification of chemical structure of substituent group, anion, cation and non-ionic ethers can be divided into.With etherificate used
The difference of agent and have methylcellulose, hydroxyethylmethylcellulose, carboxymethyl cellulose, ethyl cellulose, benzylcellulose, hydroxyl
Ethyl cellulose, hydroxypropyl methyl cellulose, cyanethyl cellulose, benzyl cyanethyl cellulose, carboxymethyl hydroxyethyl cellulose
With benzyl cellulose etc..It is larger with methylcellulose and ethyl cellulose practicability.
At present, the preparation of cellulose ether uses cotton linter or timber as raw material more.But cotton growing stage is short and takes agriculture
Family dispersing type planting patterns, is influenced big by factors such as natural conditions, peasant incomes, raw material supply is unstable, the quality good and the bad not
Together.Quality raw materials of the timber as cellulose ether are used widely in countries such as Canada, Germany, Russia.But by
Long in the growth cycle of timber, Regenerated energy force difference largely can cause climate warming using timber.Therefore, it is traditional with cotton linter
Or timber prepares cellulose ether for raw material and has some limitations.
The production technology of cellulose ether is varied, including solvent method and gas-solid method, since solvent method produces fiber
Plain ether with respect to gas-solid method produce cellulose ether, except product quality more preferably in addition to, production process is also safer, so Current Domestic
Most of producer all produces cellulose ether using solvent method.At present, cellulose ether be applied to drilling fluid when, drop dehydration effect difference with
And salt tolerance is poor.Therefore, inventing a kind of drilling fluid amphoteric cellulose ether has cellulose ether preparing technical field actively meaning
Justice.
Invention content
Present invention mainly solves the technical issues of, for cellulose ether be applied to drilling fluid when, drop dehydration effect difference and
The defects of salt tolerance is poor provides a kind of preparation method of drilling fluid amphoteric cellulose ether.
In order to solve the above-mentioned technical problem, the technical solution adopted in the present invention is：
The preparation method of a kind of drilling fluid amphoteric cellulose ether, it is characterised in that specifically preparation process is：
（1）150~160mL epoxychloropropane is added in into the three-necked flask with blender and snorkel, three-necked flask is put
In ice-water bath, front three amine gas is led into three-necked flask, starts blender stirring, ventilatory response obtains reaction product, will be anti-
Product is answered to be separated by filtration to obtain white solid product, white solid product is put into vacuum drying chamber, it is dry, obtain cation
Etherifying agent；
（2）30~35g hydroxyethyl celluloses, 120~140mL sodium hydroxide solutions and 8~10g cations are added in into reactor
Etherifying agent starts blender, is stirred to react to obtain reaction mixture, neutralizes reaction mixture with hydrochloric acid, obtain suspension, will
Suspension is placed in centrifugal treating in supercentrifuge, removes upper liquid, collects lower sediment thing, and sediment is put into baking oven and is done
It is dry, obtain cationic hydroxyethyl cellulose；
（3）40~45mL dimethylallylamine is added in into the four-hole boiling flask with condensing unit, heat temperature raising is burnt to four mouthfuls
Addition 5~7g monoxones and 60~70mL sodium hydroxide solutions, are stirred to react with 3 with magnetic stirring apparatus, obtained light yellow in bottle
Liquid；
（4）Above-mentioned light yellow liquid is put into distilling flask, heat temperature raising, distilled, obtain yellow mucus and white crystal
Mixture adds in 100~110mL absolute ethyl alcohols into the mixture of yellow mucus and white crystal, is separated by filtration to obtain pale yellow
Color mucus；
（5）The above-mentioned light yellow mucus of 40~50mL and 80~100mL deionizations are added in into the three-necked flask equipped with condensing unit
Water, then chlorine is passed through into three-necked flask, heat temperature raising, distillation continues to add in 70~80mL absolute ethyl alcohols, mistake to three-necked flask
Filter isolated thick filtrate；
（6）30~35g cationic hydroxyethyl celluloses are added in into thick filtrate, are stirred to react to obtain solid crude product, it will
The methanol solution that solid crude product is put into acetic acid impregnates, and is separated by filtration to obtain filter powder, filter powder is put into vacuum drying chamber, is done
It is dry, obtain amphoteric cellulose ether.
Step（1）The Ventilation Rate be 40~50mL/min, speed of agitator be 200~250r/min, ventilatory response
Time is 4~5h, and vacuum drying chamber set temperature is 70~80 DEG C, and drying time is 6~7h.
Step（2）The mass fraction of the sodium hydroxide solution is 15%, is stirred to react the time as 1~2h, the matter of hydrochloric acid
It is 20% to measure score, and supercentrifuge rotating speed is 2000~3000r/min, and the centrifugal treating time is 8~10min, and baking oven sets temperature
It is 60~70 DEG C to spend, and drying time is 4~5h.
Step（3）Described is 55~60 DEG C to temperature after four-hole boiling flask heat temperature raising, the quality point of sodium hydroxide solution
Number is 20%, and magnetic stirring apparatus rotating speed is 300~400r/min, is stirred to react the time as 20~30min.
Step（4）Temperature is 70~80 DEG C after the heat temperature raising, and distillation time is 1.5~2.0h.
Step（5）Ventilation Rate when being passed through chlorine is 30~35mL/min, controls reaction system in three-necked flask
PH for 6~8, temperature is 80~90 DEG C after heat temperature raising, and distillation time is 2~3h.
Step（6）Described is stirred to react the time as 30~40min, and the mass fraction of the methanol solution of acetic acid is 20%,
Soaking time is 40~50min, and the set temperature of vacuum drying chamber is in 70~80 DEG C, and drying time is 10~12h.
The beneficial effects of the invention are as follows：
（1）The present invention is passed through front three amine gas in low temperature into epoxychloropropane, is stirred to react to obtain reaction product, passes through
It filters, be dried to obtain cationic etherifying agent, after being etherified hydroxyethyl cellulose under alkaline condition with cationic etherifying agent, by centrifugation
It detaches, be dried to obtain cationic hydroxyethyl cellulose, dimethylallylamine, monoxone, sodium hydroxide solution are mixed, stirring
Light yellow liquid is obtained by the reaction, by distilling, being obtained by filtration light yellow mucus, steaming is heated after chlorine is passed through into light yellow mucus
It evaporates, adds absolute ethyl alcohol, thick filtrate filtrate is obtained by filtration, thick filtrate and cationic hydroxyethyl cellulose are stirred
Reaction, obtains solid crude product, the methanol solution immersion treatment through acetic acid filters, is dried to obtain drilling fluid amphoteric cellulose
First under alkaline condition, using the active hydroxyl groups on hydroxyethyl cellulose strand and epoxychloropropane ether occurs for ether, the present invention
Cationic hydroxyethyl cellulose ethers are obtained by the reaction, then it is the chloro- 2- hydroxypropyls diformazan ammoniums of 3- that thick filtrate, which is prepared, in change
Cationic hydroxyethyl cellulose ethers anionic is obtained amphoteric cellulose ether by acetate with thick filtrate, and of the invention two
Property cellulose ether can effectively weaken and prevent free water molecule aquation in the clay crystal layer of mud in drilling fluid, meanwhile,
The solvated layer that a large amount of anionic groups carry can improve the coagulation stability of system again, and such amphoteric cellulose ether can improve
The aquation dispersibility of clay particle in drilling fluid, improves the resistance of motion of hydrone so that cellulose ether is in drilling fluid
There is splendid drop dehydration；
（2）The number of anions and canons group is roughly equal in the amphoteric cellulose ether of the present invention, electrostatic force in strand
Only electrostatic attraction, in aqueous solution, this electrostatic attraction are acted on so that can generate association in polymeric groups and in strand
Effect, causes polymer molecule to shrink, and hydrodynamic volume reduces, and solution viscosity becomes smaller, in electrolyte solution, due to dividing
Association in subbase group and in strand is shielded by small molecule electrolyte so that the interaction energy of macromolecule and solvent
Power enhances, and molecular conformation gradually becomes to unfold, solution viscosity increase, so as to show apparent anti-polyelectrolyte solution behavior,
Make that larger consistency still can be kept when water content is higher in drilling fluid, weaken the osmosis of salting liquid, a large amount of sun from
Subbase group also has metal cation preferable repulsive interaction, avoids drilling fluid that salting-out phenomenon occurs, so as to improve both sexes fibre
Salt tolerance of the plain ether of dimension in drilling fluid, has a extensive future.
Specific embodiment
150~160mL epoxychloropropane is added in into the three-necked flask with blender and snorkel, three-necked flask is put
In ice-water bath, front three amine gas is led to the Ventilation Rate of 40~50mL/min into three-necked flask, starts blender, with 200
The rotating speed stirring of~250r/min, 4~5h of ventilatory response obtain reaction product, are separated by filtration to obtain white admittedly by reaction product
Body product, it is dry 6~7h in 70~80 DEG C of vacuum drying chamber that white solid product is put into set temperature, obtain sun from
Sub- etherifying agent；30~35g hydroxyethyl celluloses are added in into reactor, the sodium hydroxide that 120~140mL mass fractions are 15%
Solution and 8~10g cationic etherifying agents start blender, 1~2h are stirred to react with the rotating speed of 400~500r/min, obtain anti-
Answer mixture, with mass fraction be 20% hydrochloric acid reaction mixture is neutralized, obtain suspension, by suspension be placed at a high speed from
With rotating speed 8~10min of centrifugal treating of 2000~3000r/min in scheming, upper liquid is removed, collects lower sediment thing, it will be heavy
Starch is put into dry 4~5h in the baking oven that set temperature is 60~70 DEG C, obtains cationic hydroxyethyl cellulose；To with condensation
40~45mL dimethylallylamine is added in the four-hole boiling flask of device, 55~60 DEG C is heated to, adds into four-hole boiling flask
Add the sodium hydroxide solution that 5~7g monoxones and 60~70mL mass fractions are 20%, with magnetic stirring apparatus with 300~400r/
The rotating speed of min is stirred to react 20~30min, obtains light yellow liquid；Above-mentioned light yellow liquid is put into distilling flask, is heated
70~80 DEG C are warming up to, 1.5~2.0h is distilled, the mixture of yellow mucus and white crystal is obtained, to yellow mucus and white
100~110mL absolute ethyl alcohols are added in the mixture of crystal, are separated by filtration to obtain light yellow mucus；To equipped with condensing unit
Add in the above-mentioned light yellow mucus of 40~50mL and 80~100mL deionized waters in three-necked flask, then into three-necked flask with 30~
The Ventilation Rate of 35mL/min is passed through chlorine, and the pH for controlling reaction system in three-necked flask is 6~8, is heated to 80~90
DEG C, 2~3h is distilled, continues to add in 70~80mL absolute ethyl alcohols to three-necked flask, is separated by filtration to obtain thick filtrate；To sticky
30~35g cationic hydroxyethyl celluloses are added in shape filtrate, 30~40min is stirred to react and obtains solid crude product, by solid
Crude product is put into the methanol solution that mass fraction is 20% acetic acid and impregnates 40~50min, is separated by filtration to obtain filter powder, filter powder is put
Enter in the vacuum drying chamber that set temperature is 70~80 DEG C, dry 10~12h obtains amphoteric cellulose ether.
Example 1
150mL epoxychloropropane is added in into the three-necked flask with blender and snorkel, three-necked flask is placed in ice-water bath
In, front three amine gas is led to the Ventilation Rate of 40mL/min into three-necked flask, starts blender, is stirred with the rotating speed of 200r/min
It mixes, ventilatory response 4h obtains reaction product, reaction product is separated by filtration to obtain white solid product, by white solid product
It is put into the vacuum drying chamber that set temperature is 70 DEG C, dry 6h obtains cationic etherifying agent；30g hydroxyls are added in into reactor
Ethyl cellulose, the sodium hydroxide solution that 120mL mass fractions are 15% and 8g cationic etherifying agents, start blender, with
The rotating speed of 400r/min is stirred to react 1h, obtains reaction mixture, will be in reaction mixture with the hydrochloric acid that mass fraction is 20%
With obtain suspension, suspension be placed in supercentrifuge with the rotating speed centrifugal treating 8min of 2000r/min, remove upper strata
Liquid collects lower sediment thing, and sediment is put into dry 4h in the baking oven that set temperature is 60 DEG C, obtains cationic hydroxyethyl fibre
Dimension element；40mL dimethylallylamine is added in into the four-hole boiling flask with condensing unit, is heated to 55 DEG C, is burnt to four mouthfuls
Addition 5g monoxones and the sodium hydroxide solution that 60mL mass fractions are 20% in bottle, with magnetic stirring apparatus turning with 300r/min
Speed is stirred to react 20min, obtains light yellow liquid；Above-mentioned light yellow liquid is put into distilling flask, is heated to 70 DEG C,
1.5h is distilled, the mixture of yellow mucus and white crystal is obtained, is added in into the mixture of yellow mucus and white crystal
100mL absolute ethyl alcohols are separated by filtration to obtain light yellow mucus；It is above-mentioned shallow that 40mL is added in into the three-necked flask equipped with condensing unit
Yellow mucus and 80mL deionized waters, then chlorine is passed through with the Ventilation Rate of 30mL/min into three-necked flask, control three mouthfuls of burnings
The pH of reaction system is 6 in bottle, is heated to 80 DEG C, distills 2h, continues to add in 70mL absolute ethyl alcohols, filtering to three-necked flask
Isolated thick filtrate；30g cationic hydroxyethyl celluloses are added in into thick filtrate, 30min is stirred to react and obtains
Solid crude product is put into the methanol solution that mass fraction is 20% acetic acid and impregnates 40min, is separated by filtration to obtain by solid crude product
Powder is filtered, powder will be filtered and be put into the vacuum drying chamber that set temperature is 70 DEG C, dry 10h obtains amphoteric cellulose ether.
Example 2
155mL epoxychloropropane is added in into the three-necked flask with blender and snorkel, three-necked flask is placed in ice-water bath
In, front three amine gas is led to the Ventilation Rate of 45mL/min into three-necked flask, starts blender, is stirred with the rotating speed of 220r/min
It mixes, ventilatory response 4.5h obtains reaction product, and reaction product is separated by filtration to obtain white solid product, white solid is produced
Object is put into the vacuum drying chamber that set temperature is 75 DEG C, and dry 6.5, obtain cationic etherifying agent；32g is added in into reactor
Hydroxyethyl cellulose, the sodium hydroxide solution that 130mL mass fractions are 15% and 9g cationic etherifying agents, start blender, with
The rotating speed of 450r/min is stirred to react 1.5h, obtains reaction mixture, will be in reaction mixture with the hydrochloric acid that mass fraction is 20%
With obtain suspension, suspension be placed in supercentrifuge with the rotating speed centrifugal treating 9min of 2500r/min, remove upper strata
Liquid collects lower sediment thing, and sediment is put into dry 4.5h in the baking oven that set temperature is 65 DEG C, obtains cationic hydroxyethyl
Cellulose；42mL dimethylallylamine is added in into the four-hole boiling flask with condensing unit, is heated to 57 DEG C, Xiang Sikou
6g monoxones and 65mL mass fractions are added in flask as 20% sodium hydroxide solution, with magnetic stirring apparatus with 350r/min's
Rotating speed is stirred to react 25min, obtains light yellow liquid；Above-mentioned light yellow liquid is put into distilling flask, is heated to 75
DEG C, 1.7h is distilled, the mixture of yellow mucus and white crystal is obtained, is added in into the mixture of yellow mucus and white crystal
105mL absolute ethyl alcohols are separated by filtration to obtain light yellow mucus；It is above-mentioned shallow that 45mL is added in into the three-necked flask equipped with condensing unit
Yellow mucus and 90mL deionized waters, then chlorine is passed through with the Ventilation Rate of 32mL/min into three-necked flask, control three mouthfuls of burnings
The pH of reaction system is 7 in bottle, is heated to 85 DEG C, distills 2.5h, continues to add in 75mL absolute ethyl alcohols, mistake to three-necked flask
Filter isolated thick filtrate；32g cationic hydroxyethyl celluloses are added in into thick filtrate, 35min is stirred to react and obtains
To solid crude product, solid crude product is put into the methanol solution that mass fraction is 20% acetic acid and impregnates 45min, is separated by filtration
To filter powder, powder will be filtered and be put into the vacuum drying chamber that set temperature is 75 DEG C, dry 11h obtains amphoteric cellulose ether.
Example 3
160mL epoxychloropropane is added in into the three-necked flask with blender and snorkel, three-necked flask is placed in ice-water bath
In, front three amine gas is led to the Ventilation Rate of 50mL/min into three-necked flask, starts blender, is stirred with the rotating speed of 250r/min
It mixes, ventilatory response 5h obtains reaction product, reaction product is separated by filtration to obtain white solid product, by white solid product
It is put into the vacuum drying chamber that set temperature is 80 DEG C, dry 7h obtains cationic etherifying agent；35g hydroxyls are added in into reactor
Ethyl cellulose, the sodium hydroxide solution that 140mL mass fractions are 15% and 10g cationic etherifying agents, start blender, with
The rotating speed of 500r/min is stirred to react 2h, obtains reaction mixture, will be in reaction mixture with the hydrochloric acid that mass fraction is 20%
With obtain suspension, suspension be placed in supercentrifuge with the rotating speed centrifugal treating 10min of 3000r/min, remove upper strata
Liquid collects lower sediment thing, and sediment is put into dry 5h in the baking oven that set temperature is 70 DEG C, obtains cationic hydroxyethyl fibre
Dimension element；45mL dimethylallylamine is added in into the four-hole boiling flask with condensing unit, is heated to 60 DEG C, is burnt to four mouthfuls
Addition 7g monoxones and the sodium hydroxide solution that 70mL mass fractions are 20% in bottle, with magnetic stirring apparatus turning with 400r/min
Speed is stirred to react 30min, obtains light yellow liquid；Above-mentioned light yellow liquid is put into distilling flask, is heated to 80 DEG C,
2.0h is distilled, the mixture of yellow mucus and white crystal is obtained, is added in into the mixture of yellow mucus and white crystal
110mL absolute ethyl alcohols are separated by filtration to obtain light yellow mucus；It is above-mentioned shallow that 50mL is added in into the three-necked flask equipped with condensing unit
Yellow mucus and 100mL deionized waters, then chlorine is passed through with the Ventilation Rate of 35mL/min into three-necked flask, control three mouthfuls of burnings
The pH of reaction system is 8 in bottle, is heated to 90 DEG C, distills 3h, continues to add in 80mL absolute ethyl alcohols, filtering to three-necked flask
Isolated thick filtrate；35g cationic hydroxyethyl celluloses are added in into thick filtrate, 40min is stirred to react and obtains
Solid crude product is put into the methanol solution that mass fraction is 20% acetic acid and impregnates 50min, is separated by filtration to obtain by solid crude product
Powder is filtered, powder will be filtered and be put into the vacuum drying chamber that set temperature is 80 DEG C, dry 12h obtains amphoteric cellulose ether.
Comparative example
With the drilling fluid of Shandong company production with amphoteric cellulose ether as a comparison case to drilling fluid produced by the present invention with two
Drilling fluid in property cellulose ether and comparative example carries out performance detection with amphoteric cellulose ether, and testing result is as shown in table 1：
1st, test method：
Water retention test method：Example 1~3 and the cellulose ether of comparative example mean quality are weighed, is put into four identical cultures
A thin layer is paved into ware, weighs quality at this time, periodically claims its quality day by day later, water retention R is calculated as follows：R=m0-(m1-
m2)/m×100%
Note：R：Water retention, %；m0：Saturation water-absorbing resin quality, g；m1：Saturation water-absorbing resin and culture dish quality and, g；m2：Water
After point evaporation water-absorbing resin and culture dish quality and, g.
Salt tolerance test method：Cellulose ether in example 1~3 and comparative example is individually placed to molten in 15% salinity solution
Solution, measures the solubility of each cellulose ether, observes the precipitation status in each solution.
Table 1
| Test event | Example 1 | Example 2 | Example 3 | Comparative example |
| Water retention（%） | 97 | 98 | 99 | 90 |
| Water absorbent rate | 708 | 710 | 715 | 520 |
| Salt resistant character | Well, no precipitation | Well, no precipitation | Well, no precipitation | It is poor, generate more precipitation |
| Solubility（%） | 96 | 97 | 98 | 52 |
Drilling fluid produced by the present invention is good with amphoteric cellulose ether drop dehydration effect according to above-mentioned middle data, salt resistant character
Good, solubility reaches 98%, and no precipitation generates, and has broad application prospects.
Claims (7)
1. a kind of drilling fluid preparation method of amphoteric cellulose ether, it is characterised in that specifically preparation process is：
（1）150~160mL epoxychloropropane is added in into the three-necked flask with blender and snorkel, three-necked flask is put
In ice-water bath, front three amine gas is led into three-necked flask, starts blender stirring, ventilatory response obtains reaction product, will be anti-
Product is answered to be separated by filtration to obtain white solid product, white solid product is put into vacuum drying chamber, it is dry, obtain cation
Etherifying agent；
（2）30~35g hydroxyethyl celluloses, 120~140mL sodium hydroxide solutions and 8~10g cations are added in into reactor
Etherifying agent starts blender, is stirred to react to obtain reaction mixture, neutralizes reaction mixture with hydrochloric acid, obtain suspension, will
Suspension is placed in centrifugal treating in supercentrifuge, removes upper liquid, collects lower sediment thing, and sediment is put into baking oven and is done
It is dry, obtain cationic hydroxyethyl cellulose；
（3）40~45mL dimethylallylamine is added in into the four-hole boiling flask with condensing unit, heat temperature raising is burnt to four mouthfuls
Addition 5~7g monoxones and 60~70mL sodium hydroxide solutions, are stirred to react with 3 with magnetic stirring apparatus, obtained light yellow in bottle
Liquid；
（4）Above-mentioned light yellow liquid is put into distilling flask, heat temperature raising, distilled, obtain yellow mucus and white crystal
Mixture adds in 100~110mL absolute ethyl alcohols into the mixture of yellow mucus and white crystal, is separated by filtration to obtain pale yellow
Color mucus；
（5）The above-mentioned light yellow mucus of 40~50mL and 80~100mL deionizations are added in into the three-necked flask equipped with condensing unit
Water, then chlorine is passed through into three-necked flask, heat temperature raising, distillation continues to add in 70~80mL absolute ethyl alcohols, mistake to three-necked flask
Filter isolated thick filtrate；
（6）30~35g cationic hydroxyethyl celluloses are added in into thick filtrate, are stirred to react to obtain solid crude product, it will
The methanol solution that solid crude product is put into acetic acid impregnates, and is separated by filtration to obtain filter powder, filter powder is put into vacuum drying chamber, is done
It is dry, obtain amphoteric cellulose ether.
2. a kind of preparation method of drilling fluid amphoteric cellulose ether according to claim 1, it is characterised in that：
Step（1）The Ventilation Rate be 40~50mL/min, speed of agitator be 200~250r/min, the ventilatory response time
For 4~5h, vacuum drying chamber set temperature is 70~80 DEG C, and drying time is 6~7h.
3. a kind of preparation method of drilling fluid amphoteric cellulose ether according to claim 1, it is characterised in that：
Step（2）The mass fraction of the sodium hydroxide solution is 15%, is stirred to react the time as 1~2h, the quality point of hydrochloric acid
Number is 20%, and supercentrifuge rotating speed is 2000~3000r/min, and the centrifugal treating time is 8~10min, and baking oven set temperature is
60~70 DEG C, drying time is 4~5h.
4. a kind of preparation method of drilling fluid amphoteric cellulose ether according to claim 1, it is characterised in that：
Step（3）Described is 55~60 DEG C to temperature after four-hole boiling flask heat temperature raising, and the mass fraction of sodium hydroxide solution is
20%, magnetic stirring apparatus rotating speed is 300~400r/min, is stirred to react the time as 20~30min.
5. a kind of preparation method of drilling fluid amphoteric cellulose ether according to claim 1, it is characterised in that：
Step（4）Temperature is 70~80 DEG C after the heat temperature raising, and distillation time is 1.5~2.0h.
6. a kind of preparation method of drilling fluid amphoteric cellulose ether according to claim 1, it is characterised in that：
Step（5）Ventilation Rate when being passed through chlorine is 30~35mL/min, controls the pH of reaction system in three-necked flask
It is 6~8, temperature is 80~90 DEG C after heat temperature raising, and distillation time is 2~3h.
7. a kind of preparation method of drilling fluid amphoteric cellulose ether according to claim 1, it is characterised in that：
Step（6）Described is stirred to react the time as 30~40min, and the mass fraction of the methanol solution of acetic acid is 20%, is impregnated
Time is 40~50min, and the set temperature of vacuum drying chamber is in 70~80 DEG C, and drying time is 10~12h.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108864801A (en) * | 2018-07-25 | 2018-11-23 | 佛山陵朝新材料有限公司 | A kind of preparation method of salt tolerant higher suspension thickener for coating |
| CN110358519A (en) * | 2019-06-12 | 2019-10-22 | 欧志飞 | A kind of preparation method of low residue salt tolerant fracturing fluid |
| CN111214391A (en) * | 2019-11-25 | 2020-06-02 | 重庆东寰科技开发有限公司 | Amphoteric hydroxyethyl cellulose ether and preparation method thereof |
| CN111875713A (en) * | 2020-07-31 | 2020-11-03 | 董群雄 | Cellulose ether for drilling fluid and preparation method thereof |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108864801A (en) * | 2018-07-25 | 2018-11-23 | 佛山陵朝新材料有限公司 | A kind of preparation method of salt tolerant higher suspension thickener for coating |
| CN110358519A (en) * | 2019-06-12 | 2019-10-22 | 欧志飞 | A kind of preparation method of low residue salt tolerant fracturing fluid |
| CN111214391A (en) * | 2019-11-25 | 2020-06-02 | 重庆东寰科技开发有限公司 | Amphoteric hydroxyethyl cellulose ether and preparation method thereof |
| CN111214391B (en) * | 2019-11-25 | 2023-04-14 | 重庆东寰科技开发有限公司 | Amphoteric hydroxyethyl cellulose ether and preparation method thereof |
| CN111875713A (en) * | 2020-07-31 | 2020-11-03 | 董群雄 | Cellulose ether for drilling fluid and preparation method thereof |
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