CN101838333A - Method for preparing high viscosity polyanionic cellulose - Google Patents
Method for preparing high viscosity polyanionic cellulose Download PDFInfo
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- CN101838333A CN101838333A CN200910047822A CN200910047822A CN101838333A CN 101838333 A CN101838333 A CN 101838333A CN 200910047822 A CN200910047822 A CN 200910047822A CN 200910047822 A CN200910047822 A CN 200910047822A CN 101838333 A CN101838333 A CN 101838333A
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Abstract
The invention discloses a method for preparing high viscosity polyanionic cellulose, comprising the following steps with refined cotton as the cellulose raw material of alkalizing cellulose, mixing cellulose by adding an etherifying agent, etherifying cellulose, neutralizing and washing, and performing post treatment of the product; and the preparation method further comprises the step of crosslinking reaction which is performed between the step of etherifying cellulose and the step of neutralizing and washing by adding a crosslinking agent N,N'-methylene-bis-acrylamide into polyanionic cellulose to perform crosslinking reaction. The invention is a solution to the problem that the polyanionic cellulose obtained by the traditional method for preparing high viscosity polyanionic cellulose has low viscosity, poor salt tolerance and high filtration loss.
Description
Technical field
The present invention relates to a kind of preparation method of Polyanionic Cellulose, particularly a kind of preparation method of PAC HV.
Background technology
Polyanionic Cellulose (PAC) has outstanding performances such as thickening, suspension, dispersion, guarantor's dehydration, be widely used at numerous industrial sectors, mainly be used as the thickening material in the salt solution, especially in national fishing shelf and the employed mud conditioner of marine petroleum exploitation, be used for technologies such as drilling well, completion, well cementation and pressure break, show very outstanding.Along with the expansion of petroleum exploration field and the increase of drilling depth, drilling strata is increasingly sophisticated, needs various mud conditioners, so the specification of quality of Polyanionic Cellulose is improved constantly, require Polyanionic Cellulose to have high viscosity, characteristics such as salt tolerance, anticalcium and temperature resistance.It is not enough to replace homogeneity according to the product ubiquity of produced in conventional processes, and transparency rheology of solution, erosion resistance are not ideal enough, and the characteristics of salt tolerance, temperature tolerance difference.In order to improve the quality of products, people taked such as Mierocrystalline cellulose pulverize, emptying deoxidation and nitrogen-sealed, increasing solvent liquor ratio, the method such as oxidation inhibitor of adding, with obtain the polymerization degree evenly, high substitution value and the uniform product of substitution value.
In addition, little crosslinked also be Mierocrystalline cellulose and derivative functional modification thereof make things convenient for one of approach.Adopt suitable linking agent, and the control degree of crosslinking, can significantly improve the cellulosic polymerization degree, do not destroying under its active prerequisite, improve the performance of product.A series of report has been carried out in little crosslinked research to Polyanionic Cellulose at present: it is little crosslinked that oxalic dialdehyde makes Polyanionic Cellulose carry out, because oxalic dialdehyde little crosslinked mainly be to handle non-ionic celluloses ether, and unsatisfactory to the processing of anionic ether of cellulose; Also have the aluminium of use salt pair Polyanionic Cellulose to carry out little crosslinked technology, this technology not only will form macromolecular solution, and will add aluminium salt sequestrant, so this technology is convenient inadequately; The crosslinked reaction of epoxy chloropropane and hydroxyl needs carry out under higher temperature, long reaction time, and level of response is wayward, is not very desirable for the little crosslinked effect of Polyanionic Cellulose.In a word, these linking agents are in the defective that all has aspect the quality that improves Polyanionic Cellulose separately.
Publication number is CN101067002A, and the Chinese invention patent application that open day is on November 7th, 2007 discloses a kind of method that legal system is equipped with Polyanionic Cellulose of mediating.The technical scheme of this method is:
1) cellulosic alkalization: cool off kneader in advance.40%～50% sodium hydroxide solution and mass concentration are not less than 90% organic solvent and mix with certain proportion, on the Mierocrystalline cellulose that in 10～35 minutes, in kneader, constantly stirs by the jet pipe spray, the control alkalization temperature is at 5～35 ℃, alkalization time 0.5～3.0 hour, make the abundant swollen of Mierocrystalline cellulose, activation, in the hope of obtaining the uniform soda cellulose that alkalizes.
The mass ratio of Mierocrystalline cellulose and organic solvent is 1: 1～5, and organic solvent can be Virahol, ethanol, methyl alcohol, Virahol/ethanol, isopropylcarbinol etc.The mass ratio of Mierocrystalline cellulose and alkali metal hydroxide is 1: 0.4～1.2.
2) cellulosic transfer: after quaternization finishes, evenly spray Mono Chloro Acetic Acid/organic solvent solution by the acid spraying tube in the kneader under 5～35 ℃, the concentration of Mono Chloro Acetic Acid/organic solution is 50%～70%.After stirring, discharging is in plough formula reactor.Mierocrystalline cellulose and chloroacetic mass ratio are 1: 0.5～1.2, and the time that adds chloroacetic acid solution is 20～40 minutes.
3) cellulosic etherificate: material at the uniform velocity heats by adding cover in plough formula reactor, the beginning etherification reaction, and etherification reaction temperature is 45～80 ℃, the reaction times is 40～180 minutes.
4) neutralization and aftertreatment: after reaction finishes, need not cooling, directly use the washing medium washing material in and still, with excessive alkali in acetic acid or the hydrochloric acid and in the system, centrifugal, washing, drying.Washing medium can be methyl alcohol, ethanol or Virahol; Flushing can contain certain density inorganic salt or not contain inorganic salt with washing medium.
Summary of the invention
The objective of the invention is to propose a kind of preparation method of PAC HV, the problem that Polyanionic Cellulose viscosity is low, salt tolerance is poor, filter loss is high that obtains with the preparation method who solves existing Polyanionic Cellulose.
The present invention solves the problems of the technologies described above by the following technical programs, reaches purpose of the present invention.
The preparation method of PAC HV, this preparation method are cellulosic material with the purified cotton, and the step that comprises has:
A) cellulosic alkalization;
B) cellulosicly mix with etherifying agent;
C) cellulosic etherificate;
D) neutralization washing;
E) aftertreatment of product;
Described preparation method also comprises the crosslinking reaction step, described crosslinking reaction step is carried out in cellulosic etherificate of described step c) and described step d) and between the washing, described crosslinking reaction step is with linking agent N, and N '-methylene-bisacrylamide joins and carries out crosslinking reaction in the Polyanionic Cellulose.
The present invention has selected N, N '-methylene-bisacrylamide carries out little crosslinked to Polyanionic Cellulose (PAC), because this cross linker active is than higher, fast with Mierocrystalline cellulose hydroxyl reaction speed, reaction is control easily, so N, N '-methylene-bisacrylamide carries out little crosslinked more effective as linking agent to Polyanionic Cellulose, this little crosslinked homogeneity that the Polyanionic Cellulose substituting group distributes that improved has improved the viscosity of Polyanionic Cellulose.This case the contriver also be surprised to find that, uses N, and N '-methylene-bisacrylamide has also improved the application performance of Polyanionic Cellulose as linking agent, has particularly improved Polyanionic Cellulose filter loss, salt tolerance.Use N, N '-methylene-bisacrylamide carries out the PAC HV that crosslinking reaction obtains as linking agent, compares with blank sample, about viscosity is doubled, and filter loss is no more than 15ml, and the apparent viscosity in saturated brine is higher than 32mpas.Present method adopts crosslinked technological process after the first carboxymethylation, has successfully prepared a kind of PAC HV, and this product belongs to the Polyanionic Cellulose product, can be used for fields such as petroleum drilling fluid and oil production.
First optimized technical scheme of the present invention is, the temperature of described crosslinking reaction is controlled at 40 ℃-65 ℃, and the time of described crosslinking reaction is controlled at 30min-80min, and the amount of described linking agent is controlled to be the 0.75%-1.5% of purified cotton weight.
Second optimized technical scheme of the present invention is in the cellulosic alkalization of described step a), to lead to N
2The protection Mierocrystalline cellulose.This case contriver tests discovery, logical N
2The protection Mierocrystalline cellulose has reduced cellulosic oxidative degradation, helps to improve the viscosity of product, also helps the relatively plain ether of homogeneous fibre of preparation, logical N in the technical program
2Protection is to N
2Pressure does not have certain particular requirement, as long as reaction can be reacted under protection of inert gas.
The 3rd optimized technical scheme of the present invention is, described preparation method also comprises cellulosic double alkalisation step, described cellulosic double alkalisation step described step b) cellulosic mix with etherifying agent and the cellulosic etherificate of described step c) between carry out, the temperature of described cellulosic double alkalisation step is 15 ℃-40 ℃, alkalization time is 10min-30min, the weight of the used liquid caustic soda of described cellulosic double alkalisation step accounts for the 10%-40% of the gross weight of cellulosic alkalization of described step a) and the used liquid caustic soda of described cellulosic double alkalisation step, and the concentration of liquid caustic soda is 45%-52%.Double alkalisation helps the Mierocrystalline cellulose alkalization fully, the substitution value that helps to improve reaction uniformity and improve product.Further, in described cellulosic double alkalisation step, logical N
2The protection Mierocrystalline cellulose.
Description of drawings
Fig. 1 is the preparation method's of the PAC HV described in the embodiment a schema.
Embodiment
Further specify technical scheme of the present invention below in conjunction with drawings and Examples.
Referring to Fig. 1.The preparation method of PAC HV specifically may further comprise the steps:
1), premix: in kneader, add solid caustic soda, liquid caustic soda and alcohol, premix 10min-30min is dissolved in liquid caustic soda and the alcohol solid caustic soda basically.Adopting the alkali of two kinds of physical forms, mainly is in order to control the moisture in the reaction, to reduce the generation of side reaction.
2), feed intake: premix is put into the purified cotton that has torn up in the kneader after finishing, and the mean polymerisation degree of purified cotton is 2000-4000.
3), cellulosic alkalization: the mode by spray joins liquid caustic soda and alcohol in the kneader, carries out cellulosic alkalization, and logical cooling water control temperature is led to N at 15 ℃-40 ℃ in the whole alkalization process
2Protection, alkalization time is 30min-80min.
4), cellulosicly mix with etherifying agent: the mode by spray joins the Mono Chloro Acetic Acid spirituous solution in the kneader, mediates 10min-30min, and the concentration of Mono Chloro Acetic Acid spirituous solution is 65%-75%, and the mass ratio of Mono Chloro Acetic Acid and purified cotton is 0.95-1.2.
5), cellulosic double alkalisation: the mode by spray joins liquid caustic soda in the kneader, carries out cellulosic double alkalisation, and logical cooling water control temperature is led to N at 15 ℃-40 ℃ in the whole double alkalisation process
2Protection, alkalization time is 10min-30min, the weight of the used liquid caustic soda of cellulosic double alkalisation step accounts for the 10%-40% of the gross weight of cellulosic alkalization and the used liquid caustic soda of cellulosic double alkalisation step.
6), cellulosic etherificate: the temperature of etherification reaction is controlled at 70 ℃-85 ℃, and the time of etherification reaction is controlled at 30min-90min.
7), crosslinking reaction: etherification reaction finishes the back and reduces temperature about 55 ℃, add linking agent N, the N-methylene-bisacrylamide, the consumption of linking agent is the 0.75%-1.5% of purified cotton quality, then temperature is controlled under 40 ℃-65 ℃ and carries out crosslinking reaction, reaction times is controlled at 30min-80min, is cooled to afterwards below 55 ℃.
8), neutralization washing: etherification reaction joins the etherificate product in the alcohol of 65%-85% after finishing, and adds the appropriate hydrochloric acid adjust pH at 6.5-9.0, and washing is centrifugal.
9), the aftertreatment of product: through three washings, three times centrifugal, and processes such as final product drying, pulverizing obtain white or micro-yellow powder material, are target product.
Reaction ethanol concn 〉=92% of using in this invention, the washing ethanol concn is 65%-85%, liquid caustic soda concentration is 45%-52%.
The mass ratio of reaction alcohol and purified cotton is 1.5-2.5; The mass ratio of Mono Chloro Acetic Acid and purified cotton is 0.95-1.2; Used liquid caustic soda is a sodium hydroxide solution, and solid caustic soda is a sodium hydroxide, and total sodium hydroxide is 1.95-2.1 with the ratio of chloroacetic amount of substance in liquid caustic soda and the solid caustic soda.
The method for analyzing performance of products obtained therefrom of the present invention:
The viscosimetric analysis of product, the massfraction of formulated product are 1% the aqueous solution, with its viscosity of Brookfield viscometer determining; Substitution value, pH value, Cl
-Content, the sticking ratio of salt, moisture content are analyzed according to the GB1904-2005 testing standard.
Application performance is tested according to the testing method of following high viscosity PAC.
The testing method of high viscosity PAC:
1. the test of apparent viscosity
1.425gPAC is joined in the saturated brine of 350ml lentamente, stir 20min with universal mixer, in 25 ℃ of following standing over night of room temperature, with its rheological property of FANN35 viscosity instrumentation, 1/2 of reading is the apparent viscosity of sample.
2. the test of filter loss
Be made into the solution of 10ppb with deionized water or distilled water and sodium bentonite, sodium bentonite slowly must be added to the water, stir 1h, standing over night.Time spent restir 10min gets 350ml solution, adds 11.25gKCl, 7.5g sea salt, 10.5g are estimated soil, a kind of material of every adding, stir 5min, adjust pH value to 9-9.5, when agitator reaches 8000 rev/mins with NaOH, slowly add 0.75gPAC, stir 20min with universal mixer again, in 25 ℃ of following standing over night of room temperature, behind the restir 5min, pour at once in the API room temperature filter press, add 100psi pressure, survey the amount of filtrate behind the 30min, be filter loss.
Comparative Examples 1
The preparation method of PAC HV as a comparison specifically may further comprise the steps:
1), premix: in kneader, add 626g concentration and be 49% liquid caustic soda and 1400ml concentration and be 96% alcohol and the solid caustic soda of 170g, premix 25min is dissolved in liquid caustic soda and the alcohol solid caustic soda basically.
2), feed intake: premix is put into the 1200g purified cotton that has torn up in the kneader after finishing, and the mean polymerisation degree of purified cotton is 2000-4000.
3), cellulosic alkalization: the mode by spray is that 49% liquid caustic soda and 1000ml concentration are that 96% alcohol joins in the kneader with 600g concentration, carries out cellulosic alkalization, in the whole alkalization process logical cooling water control temperature at 15 ℃-40 ℃, logical N
2Protection, alkalization time is 55min.
4), cellulosicly mix with etherifying agent: the mode by spray is that 70% Mono Chloro Acetic Acid spirituous solution joins in the kneader with 1714g concentration, mediates 10min.
5), cellulosic double alkalisation: the mode by spray is that 49% liquid caustic soda joins in the kneader with 500g concentration, carries out cellulosic double alkalisation, in the whole double alkalisation process logical cooling water control temperature at 15 ℃-40 ℃, logical N
2Protection, alkalization time is 10min.
6), cellulosic etherificate: double alkalisation finishes the slow elevated temperature in back and carries out etherification reaction, and the temperature of etherification reaction is controlled at 70 ℃-85 ℃, and the time of etherification reaction is controlled at 40min.
7), neutralization washing: etherification reaction is cooled to below 60 ℃ after finishing, and it is in 68% the alcohol that 500g etherificate product is joined 1800ml concentration, adds the appropriate hydrochloric acid adjust pH at 6.5-9.0, and washing is centrifugal.
8), the aftertreatment of product: through three washings, three times centrifugal, and processes such as final product drying, pulverizing obtain white or micro-yellow powder material, are blank sample.
It is 1% the aqueous solution that blank sample is made massfraction, with its viscosity of Brookfield viscometer determining; Application performance is tested according to the testing method of above-mentioned high viscosity PAC; All the other projects are analyzed according to the GB1904-2005 testing standard; The result is as follows:
Table 1: the performance analysis of Comparative Examples 1 blank sample
Embodiment 2
The preparation method of PAC HV specifically may further comprise the steps:
1), premix: in kneader, add 644g concentration and be 48.5% liquid caustic soda and 1300ml concentration and be 93% alcohol and the solid caustic soda of 170g, premix 20min under 20 ℃ of-40 ℃ of temperature is dissolved in liquid caustic soda and the alcohol solid caustic soda basically.
2), feed intake: premix is put into the 1200g purified cotton that has torn up in the kneader after finishing, and the mean polymerisation degree of purified cotton is 2000-4000.
3), cellulosic alkalization: the mode by spray is that 48.5% liquid caustic soda and 1200ml concentration are that 93% alcohol joins in the kneader with 600g concentration, carries out cellulosic alkalization, in the whole alkalization process logical cooling water control temperature at 15 ℃-40 ℃, logical N
2Protection, alkalization time is 50min.
4), cellulosicly mix with etherifying agent: the mode by spray is that 70% Mono Chloro Acetic Acid spirituous solution joins in the kneader with 1714g concentration, mediates 20min.
5), cellulosic double alkalisation: the mode by spray is that 48.5% liquid caustic soda joins in the kneader with 500g concentration, carries out cellulosic double alkalisation, in the whole double alkalisation process logical cooling water control temperature at 15 ℃-40 ℃, logical N
2Protection, alkalization time is 15min.
6), cellulosic etherificate: heat up behind the double alkalisation and carry out etherification reaction, the temperature of etherification reaction is controlled at 70 ℃-85 ℃, and the time of etherification reaction is controlled at 40min.
7), crosslinking reaction: etherification reaction finishes the back and reduces temperature about 55 ℃, add 12g linking agent N,N methylene bis acrylamide, then temperature is controlled under 45 ℃-60 ℃ and carries out crosslinking reaction, reaction times is controlled at 55min, is cooled to afterwards below 55 ℃.
8), neutralization washing: after etherification reaction finished, it was in 72% the alcohol that 508g etherificate product is joined 1800ml concentration, adds the appropriate hydrochloric acid adjust pH at 6.5-9.0, and washing is centrifugal.
9), the aftertreatment of product: through three washings, three times are centrifugal, final product drying, processes such as pulverizing obtain white or micro-yellow powder material, are target product.
It is 1% the aqueous solution that the target product that present embodiment is made is made massfraction, with its viscosity of Brookfield viscometer determining; Application performance is tested according to the testing method of above-mentioned high viscosity PAC; All the other projects are analyzed according to GB 1904-2005 testing standard; Analytical results is as follows:
Table 2: the performance analysis of the target product of present embodiment
Embodiment 3
The preparation method of PAC HV specifically may further comprise the steps:
1), premix: in kneader, add 626g concentration and be 49.5% liquid caustic soda and 1200ml concentration and be 95% alcohol and the solid caustic soda of 170g, premix 15min under 20 ℃ of-40 ℃ of temperature is dissolved in liquid caustic soda and the alcohol solid caustic soda basically.
2), feed intake: premix is put into the 1200g purified cotton that has torn up in the kneader after finishing, and the mean polymerisation degree of purified cotton is 2000-4000.
3), cellulosic alkalization: the mode by spray is that 49.5% liquid caustic soda and 1200ml concentration are that 95% alcohol joins in the kneader with 600g concentration, carries out cellulosic alkalization, in the whole alkalization process logical cooling water control temperature at 15 ℃-40 ℃, logical N
2Protection, alkalization time is 60min.
4), cellulosicly mix with etherifying agent: the mode by spray is that 71% Mono Chloro Acetic Acid spirituous solution joins in the kneader with 1700g concentration, mediates 10min.
5), cellulosic double alkalisation: the mode by spray is that 49.5% liquid caustic soda joins in the kneader with 500g concentration, carries out cellulosic double alkalisation, in the whole double alkalisation process logical cooling water control temperature at 15 ℃-40 ℃, logical N
2Protection, alkalization time is 20min.
6), cellulosic etherificate: heat up and carry out etherification reaction in the alkalization back, the temperature of etherification reaction is controlled at 70 ℃-85 ℃, and the time of etherification reaction is controlled at 50min.
7), crosslinking reaction: etherification reaction finishes the back and reduces temperature about 55 ℃, add 9g linking agent N,N methylene bis acrylamide, then temperature is controlled under 45 ℃-60 ℃ and carries out crosslinking reaction, reaction times is controlled at 60min, is cooled to afterwards below 55 ℃.
8), neutralization washing: after etherification reaction finished, it was in 70% the alcohol that 522g etherificate product is joined 2000ml concentration, adds the appropriate hydrochloric acid adjust pH at 6.5-9.0, and washing is centrifugal.
9), the aftertreatment of product: through three washings, three times are centrifugal, final product drying, processes such as pulverizing obtain white or micro-yellow powder material, are target product.
The target product that present embodiment is made is made the aqueous solution of massfraction 1%, with its viscosity of Brookfield viscometer determining; Application performance is tested according to the testing method of above-mentioned high viscosity PAC; All the other projects are analyzed according to the GB1904-2005 testing standard; Analytical results is as follows:
Table 3: the performance analysis of the target product of present embodiment
Those of ordinary skill in the art will be appreciated that, above embodiment is used for illustrating the present invention, and be not to be used as limitation of the invention, as long as in connotation scope of the present invention, all will drop in claims scope of the present invention variation, the modification of the above embodiment.
Claims (5)
1. the preparation method of PAC HV, this preparation method is a cellulosic material with the purified cotton, the step that comprises has:
A) cellulosic alkalization;
B) cellulosicly mix with etherifying agent;
C) cellulosic etherificate;
D) neutralization washing;
E) aftertreatment of product;
It is characterized in that: described preparation method also comprises the crosslinking reaction step, described crosslinking reaction step is carried out in cellulosic etherificate of described step c) and described step d) and between the washing, described crosslinking reaction step is with linking agent N, and N '-methylene-bisacrylamide joins and carries out crosslinking reaction in the Polyanionic Cellulose.
2. the preparation method of PAC HV according to claim 1, it is characterized in that: the temperature of described crosslinking reaction is controlled at 40 ℃-65 ℃, the time of described crosslinking reaction is controlled at 30min-80min, and the amount of described linking agent is controlled to be the 0.75%-1.5% of purified cotton weight.
3. the preparation method of PAC HV according to claim 1 is characterized in that: in the cellulosic alkalization of described step a), lead to N
2The protection Mierocrystalline cellulose.
4. according to claim 1, the preparation method of 2 or 3 described PAC HV, it is characterized in that: described preparation method also comprises cellulosic double alkalisation step, described cellulosic double alkalisation step described step b) cellulosic mix with etherifying agent and the cellulosic etherificate of described step c) between carry out, the temperature of described cellulosic double alkalisation step is 15 ℃-40 ℃, alkalization time is 10min-30min, the weight of the used liquid caustic soda of described cellulosic double alkalisation step accounts for the 10%-40% of the gross weight of cellulosic alkalization of described step a) and the used liquid caustic soda of described cellulosic double alkalisation step, and the concentration of described liquid caustic soda is 45%-52%.
5. the preparation method of PAC HV according to claim 4 is characterized in that: in described cellulosic double alkalisation step, lead to N
2The protection Mierocrystalline cellulose.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103087202A (en) * | 2012-12-20 | 2013-05-08 | 杭州弘博化工有限公司 | Preparation method of polyanionic cellulose with ultrahigh viscosity for water-based drilling fluid |
| CN116375892A (en) * | 2023-04-04 | 2023-07-04 | 徐州创力纤维有限公司 | Preparation method of polyanionic cellulose |
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2009
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103087202A (en) * | 2012-12-20 | 2013-05-08 | 杭州弘博化工有限公司 | Preparation method of polyanionic cellulose with ultrahigh viscosity for water-based drilling fluid |
| CN116375892A (en) * | 2023-04-04 | 2023-07-04 | 徐州创力纤维有限公司 | Preparation method of polyanionic cellulose |
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Application publication date: 20100922 |