CN105254769B - A kind of method of technology of preparing level sodium carboxymethylcellulose - Google Patents
A kind of method of technology of preparing level sodium carboxymethylcellulose Download PDFInfo
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- CN105254769B CN105254769B CN201510824422.5A CN201510824422A CN105254769B CN 105254769 B CN105254769 B CN 105254769B CN 201510824422 A CN201510824422 A CN 201510824422A CN 105254769 B CN105254769 B CN 105254769B
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Abstract
The invention belongs to chemical fields, and in particular to a kind of method of technology of preparing level sodium carboxymethylcellulose.Technical problem to be solved by the invention is to provide a kind of methods of technology of preparing level sodium carboxymethylcellulose, comprising the following steps: alcohol and sodium hydrate aqueous solution a, are mixed to obtain mixed liquor；B, quaternization is carried out after mixing mixed liquor and cellulosic material；C, etherifying agent is added in the material after step b quaternization and carries out etherification reaction；D, alcohol and sodium hydrate aqueous solution are mixed into obtain mixed liquor；E, quaternization is carried out after mixing the material after the mixed liquor of step d and step c etherification reaction；F, oxidant is added in material after step d alkalizes, alcohol carries out purification viscosity reduction.This method can prepare the technology level sodium carboxymethylcellulose of low viscosity, and purity can achieve 75% or more, and being etherified efficiency can be up to 70% or more.
Description
Technical field
The invention belongs to chemical fields, and in particular to a kind of method of technology of preparing level sodium carboxymethylcellulose.
Background technique
The low viscous sodium carboxymethylcellulose of technical grade is domestic appearance petroleum level sodium carboxymethylcellulose product type earlier,
Suitable for shallow well and deep-well shallow-layer area, so dosage is very big.The low viscous sodium carboxymethylcellulose of technical grade drilling fluid, cementing fluid and
Landing dehydration acts in fracturing fluid, to have the function that retaining wall, protect drill bit, prevent mud loss, improve bit speed.
The prior art generally uses an alkalization method to prepare sodium carboxymethylcellulose, but reacts etherificate efficiency on 65% left side
The right side, product performance index apparent viscosity in 80~90mpa.s, are in the index upper limit, are not able to satisfy existing oil field pair substantially
The demand of sodium carboxymethylcellulose.
Summary of the invention
For the problems of existing sodium carboxymethylcellulose, goal of the invention of the invention, which is to provide, a kind of prepares skill
The method of art level sodium carboxymethylcellulose.The carboxymethyl cellulose that the etherificate efficiency of this method is up to 70%, and is prepared
The viscosity of sodium is lower than 80mpa.s.
Technical problem to be solved by the invention is to provide a kind of methods of technology of preparing level sodium carboxymethylcellulose.The party
Method the following steps are included:
A, it prepares mixed liquor: 225~270 parts of alcohol and 100~140 parts of sodium hydrate aqueous solutions being mixed, temperature is controlled
It is 35~50 DEG C；1.5~6 parts of hydrogen peroxide are added thereto again and obtain mixed liquor controlled at 35~50 DEG C；
B, alkalize: control reaction unit temperature is 25 DEG C~45 DEG C, by the wood pulp of 50~70 parts of cp≤40mpa.s or bamboo
It starches, the mixed liquor of step a is added in reaction unit and carries out quaternization；Charging start to alkalization finishing control temperature be 25~
65 DEG C, the time after charging terminates to alkalization is 70~110min；
C, it is etherified: 70~90 parts of etherifying agent being added in the material that step b reaction terminates and carries out etherification reaction；Charging
Start to etherificate finishing control temperature to be 40~65 DEG C, the time that charging starts to terminate to etherificate is 35~65min；The etherificate
Agent is concentration 73.0~75.0% (w/w) monoxone alcoholic solution；
D, mixed liquor is prepared again: 80~120 parts of alcohol and 35~50 parts of sodium hydrate aqueous solutions are mixed, control mixing
Liquid temperature is 35~50 DEG C, obtains mixed liquor；
E, it alkalizes: the mixed liquor of step d being added in the material that step c reaction terminates and carries out quaternization；Charging is opened
Begin to alkalization finishing control temperature to be 40~70 DEG C, the time that charging starts to terminate to alkalization is 10~20min；It is warming up to 76 again
~78 DEG C of 25~35min of constant temperature；It is cooled to 50 DEG C or less again；
F, it refines viscosity reduction: oxidant, 1750~2500 parts of alcohol being added in the material that step e reaction terminates, stirring
It is centrifuged, dries afterwards, crushing, packaging；The oxidant is 3~10 parts of hydrogen peroxide or 1.5~10 parts of sodium hypochlorite；
Above-mentioned number indicates the mole of each raw material；If the raw material is solution, number if, indicates the mole of its solute.
Preferably, in the method and step a of above-mentioned technology of preparing level sodium carboxymethylcellulose, the concentration of the alcohol is 90~
95% (v/v)；The concentration of the sodium hydrate aqueous solution is 48.0~50.0% (w/w).
Preferably, in the method and step a of above-mentioned technology of preparing level sodium carboxymethylcellulose, the mass fraction of the hydrogen peroxide
It is 27.5% or more, the hydrogen peroxide that is added is that 5~10min before carrying out step b is added.
Preferably, in the method and step b of above-mentioned technology of preparing level sodium carboxymethylcellulose, the charging starts to charging to tie
The time of beam is 10~15min.
Preferably, in the method and step c of above-mentioned technology of preparing level sodium carboxymethylcellulose, the etherifying agent is with quality point
>=97.5% monoxones of number are that solute, 90~95% (v/v) alcohol are formulated for solvent.
Preferably, in the method and step c of above-mentioned technology of preparing level sodium carboxymethylcellulose, the etherification reaction are as follows: will
70~90 parts of etherifying agent be added in 20~25min in the material of step b after reaction at 40~50 DEG C stirring 5~
10min is warming up to 60~65 DEG C of 15~20min of constant temperature then at 5~10min.
Preferably, in the method and step d of above-mentioned technology of preparing level sodium carboxymethylcellulose, the concentration of the alcohol is 90~
95% (v/v)；The concentration of the sodium hydrate aqueous solution is 48.0~50.0% (w/w).
Preferably, described to be warming up to 76~78 DEG C and be in the method and step e of above-mentioned technology of preparing level sodium carboxymethylcellulose
76~78 DEG C are warming up in 15~20min.
Preferably, in the method and step f of above-mentioned technology of preparing level sodium carboxymethylcellulose, the alcohol concentration be 65~
75% (v/v).
Preferably, in the method and step f of above-mentioned technology of preparing level sodium carboxymethylcellulose, the mixing time be 5~
30min。
The method of the present invention can make etherificate efficiency reach 70% or more, improve 5% or more, also, this than original method
The apparent viscosity for the technology level sodium carboxymethylcellulose that inventive method is prepared is lower than 80mps.
Specific embodiment
A kind of method of technology of preparing level sodium carboxymethylcellulose, comprising the following steps:
A, prepare mixed liquor: by 225~270 parts of concentration be 90~95% (v/v) alcohol and 100~140 parts of concentration are
48.0~50.0% (w/w) sodium hydrate aqueous solutions mix, controlled at 35~50 DEG C；It is added 1.5~6 parts pairs thereto again
Oxygen water obtains mixed liquor controlled at 35~50 DEG C；
B, alkalize: control reaction unit temperature is 25 DEG C~45 DEG C, by the wood pulp or bamboo pulp of 50~70 parts of cp≤40mpa.s
It is added in reaction unit, while the mixed liquor of step a is added in reaction unit in 10~15min and alkalize instead
It answers；Charging start to alkalization finishing control temperature be 25~65 DEG C, charging terminate to alkalization after time be 70~
110min；
C, it is etherified: 70~90 parts of etherifying agent is added in the material of step b after reaction in 15~25min
5~10min is stirred at 40~50 DEG C, is warming up to 60~65 DEG C of 10~20min of constant temperature then at 5~10min；The etherifying agent with
Mass fraction >=97.5% monoxone is that solute, 90~95% (v/v) alcohol are formulated for solvent, and the concentration of etherifying agent is
73.0~75.0% (w/w)；
D, prepare mixed liquor again: by 80~120 parts of concentration be 90~95% (v/v) alcohol and 35~50 parts of concentration are
48.0~50.0% (w/w) sodium hydrate aqueous solutions mix, and control mixeding liquid temperature is 35~50 DEG C, obtain mixed liquor；
E, it alkalizes: the mixed liquor of step d being added in the material that step c reaction terminates and carries out quaternization；Charging is opened
Begin to alkalization finishing control temperature to be 40~70 DEG C, the time that charging starts to terminate to alkalization is 10~20min；Again 15~
It is warming up to 76~78 DEG C of 25~35min of constant temperature in 20min, then is cooled to 50 DEG C or less；
F, it refines viscosity reduction: being the mixing of 65~75% (v/v) alcohol by oxidant and 1750~2500 parts of concentration, by step e
The material that reaction terminates is added thereto, and is centrifuged, drying, is crushed, packaging after 5~30min of stirring；The oxidant is 3
~10 parts of hydrogen peroxide or 1.5~10 parts of sodium hypochlorite；Above-mentioned number indicates the mole of each raw material；If the raw material is solution,
Number then indicates the mole of its solute.
In the method for the present invention, such as: 1) when raw material is solution, as 100~140 parts of sodium hydroxides in step a are water-soluble
Liquid indicates that the mole for the sodium hydrate solid that purity is 100% is 100~140 parts, if used solid sodium hydroxide
Purity is not 100%, then being then added in corresponding water with regard to weighing again after being converted, being configured to respective concentration
Sodium hydrate aqueous solution；2) when raw material sheet is as liquid, such as 1.5~10 parts of sodium hypochlorite in step f, pure secondary chlorine is indicated
The mole of sour sodium is 1.5~10 parts.
Embodiment 1
(1), it prepares mixed liquor: being that 93% (v/v) alcohol and the 48.34% of 115 parts (w/w) liquid alkaline are mixed by 250 parts of concentration
Mixed liquor is closed to obtain, and controlling mixeding liquid temperature is 40 DEG C~45 DEG C；3.5 parts of hydrogen peroxide are added alkali wine and mixed by 5min before feeding intake
In liquid, temperature control is at 40 DEG C~45 DEG C after mixing；
(2), alkalize: control mediates 40 DEG C~45 DEG C of built-in temperature, by the fiber of cp=26mpa.s in 10~12min
In 63 parts of addition kneaders of plain wood pulp, while mixed liquor prepared by step (1) being added in kneader by spray tube, is mixed
12~15min of time is added in liquid, and the quaternization time (not including charging time) is 100min, controls 40 DEG C of quaternization temperature
~65 DEG C；
(3), be etherified: 74.04% (w/w) monoxone alcoholic solution 75 is added by spray tube in the material after quaternization
Part, the addition time is 20min, stirs 5min later；It is heated up again by 5min, until 61~63 DEG C of constant temperature 15min；Etherification reaction temperature
Degree is 40 DEG C~63 DEG C；
(4), mixed liquor is prepared again: 100 parts of 93% (v/v) alcohol and the 48.34% of 40 parts (w/w) liquid alkaline are mixed
Mixed liquor is obtained, and controlling mixeding liquid temperature is 40 DEG C~45 DEG C；
(5), alkalize: into the material after etherification reaction by spray tube addition step (4) solution, the addition time is
5min is warming up to 76 DEG C~78 DEG C constant temperature 30min by 15min after stirring 5min, is cooled to 50 DEG C or less entrance and refined
Journey；
(6), it refines viscosity reduction process: 73% 2100 parts of (v/v) alcohol being added in washing kettle, is then slowly added into 3.5 parts
Hydrogen peroxide stirs evenly；Step (5) material is put into washing kettle after mixing, stirring 20min carried out after viscosity reduction from
The heart takes off liquid, drying, crushing, packs to obtain the low viscous sodium carboxymethylcellulose of finished product technical grade.
The technology level sodium carboxymethylcellulose that the method for the present invention is prepared is compared using national standard GB/T 5005-2010
Properties of product (being shown in Table 2) of the sodium carboxymethylcellulose that properties of product (being shown in Table 1) and existing method are prepared compares.
Table 1
Table 2
It in summary it can be seen, the technology level sodium carboxymethylcellulose viscosity of the method for the present invention preparation is lower, and etherificate rate
Up to 70% or more, so that the preparation for technology level sodium carboxymethylcellulose provides a more efficient way.
Claims (9)
1. a kind of method of technology of preparing level sodium carboxymethylcellulose, it is characterised in that: the following steps are included:
A, it prepares mixed liquor: 225~270 parts of alcohol and 100~140 parts of sodium hydrate aqueous solutions being mixed, controlled at 35
~50 DEG C；1.5~6 parts of hydrogen peroxide are added thereto again and obtain mixed liquor controlled at 35~50 DEG C；
B, alkalize: control reaction unit temperature is 25 DEG C~45 DEG C, by the wood pulp or bamboo pulp, step of 50~70 parts of cp≤40mpa.s
The mixed liquor of rapid a, which is added in reaction unit, carries out quaternization；Charging starts to alkalization finishing control temperature to be 25~65 DEG C,
Time after charging terminates to alkalization is 70~110min；
C, it is etherified: 70~90 parts of etherifying agent being added in the material that step b reaction terminates and carries out etherification reaction；Charging starts
It is 40~65 DEG C to etherificate finishing control temperature, the time that charging starts to terminate to etherificate is 35~65min；The etherifying agent is
73.0~75.0% monoxone alcoholic solution of mass concentration；
D, mixed liquor is prepared again: 80~120 parts of alcohol and 35~50 parts of sodium hydrate aqueous solutions being mixed, mixed liquor temperature is controlled
Degree is 35~50 DEG C, obtains mixed liquor；
E, it alkalizes: the mixed liquor of step d being added in the material that step c reaction terminates and carries out quaternization；Charging start to
The finishing control temperature that alkalizes is 40~70 DEG C, and the time that charging starts to terminate to alkalization is 10~20min；Again in 15~20min
Inside it is warming up to 76~78 DEG C of 25~35min of constant temperature；It is cooled to 50 DEG C or less again；
F, refine viscosity reduction: by oxidant, 1750~2500 parts of alcohol be added to step e reaction terminate material in, after stirring from
The heart, drying, crushing, packaging；The oxidant is 3~10 parts of hydrogen peroxide or 1.5~10 parts of sodium hypochlorite；
Above-mentioned number indicates the mole of each raw material；If the raw material is solution, number if, indicates the mole of its solute.
2. the method for technology of preparing level sodium carboxymethylcellulose according to claim 1, it is characterised in that: in step a, institute
The volumetric concentration for stating alcohol is 90~95%；The mass concentration of the sodium hydrate aqueous solution is 48.0~50.0%.
3. the method for technology of preparing level sodium carboxymethylcellulose according to claim 1, it is characterised in that: in step a, institute
The mass fraction for stating hydrogen peroxide is 27.5% or more, and the hydrogen peroxide that is added is that 5~10min before carrying out step b is carried out
Addition.
4. the method for technology of preparing level sodium carboxymethylcellulose according to claim 1, it is characterised in that: in step b, institute
Stating the time that charging starts to terminate to charging is 10~15min.
5. the method for technology of preparing level sodium carboxymethylcellulose according to claim 1, it is characterised in that: in step c, institute
The etherifying agent stated is that solvent is formulated by solute, 90~95% alcohol of volume fraction of mass fraction >=97.5% monoxone.
6. the method for technology of preparing level sodium carboxymethylcellulose according to claim 1, it is characterised in that: in step c, institute
The etherification reaction stated are as follows: 70~90 parts of etherifying agent is added in the material of step b after reaction in 20~25min
5~10min is stirred at 40~50 DEG C, is warming up to 60~65 DEG C of 15~20min of constant temperature then at 5~10min.
7. the method for technology of preparing level sodium carboxymethylcellulose according to claim 1, it is characterised in that: in step d, institute
The volumetric concentration for stating alcohol is 90~95%；The mass concentration of the sodium hydrate aqueous solution is 48.0~50.0%.
8. the method for technology of preparing level sodium carboxymethylcellulose according to claim 1, it is characterised in that: in step f, institute
The alcohol by volume concentration stated is 65~75%.
9. the method for technology of preparing level sodium carboxymethylcellulose according to claim 1, it is characterised in that: in step f, institute
The mixing time stated is 5~30min.
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| CN112194731A (en) * | 2020-09-21 | 2021-01-08 | 湖州展望药业有限公司 | Injection-grade low-viscosity sodium carboxymethylcellulose and preparation method thereof |
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