CN109265695A - A kind of preparation method and application thickening modified xantham gum - Google Patents
A kind of preparation method and application thickening modified xantham gum Download PDFInfo
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- CN109265695A CN109265695A CN201810974799.2A CN201810974799A CN109265695A CN 109265695 A CN109265695 A CN 109265695A CN 201810974799 A CN201810974799 A CN 201810974799A CN 109265695 A CN109265695 A CN 109265695A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G81/00—Macromolecular compounds obtained by interreacting polymers in the absence of monomers, e.g. block polymers
- C08G81/02—Macromolecular compounds obtained by interreacting polymers in the absence of monomers, e.g. block polymers at least one of the polymers being obtained by reactions involving only carbon-to-carbon unsaturated bonds
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- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B37/00—Preparation of polysaccharides not provided for in groups C08B1/00 - C08B35/00; Derivatives thereof
- C08B37/0006—Homoglycans, i.e. polysaccharides having a main chain consisting of one single sugar, e.g. colominic acid
- C08B37/0024—Homoglycans, i.e. polysaccharides having a main chain consisting of one single sugar, e.g. colominic acid beta-D-Glucans; (beta-1,3)-D-Glucans, e.g. paramylon, coriolan, sclerotan, pachyman, callose, scleroglucan, schizophyllan, laminaran, lentinan or curdlan; (beta-1,6)-D-Glucans, e.g. pustulan; (beta-1,4)-D-Glucans; (beta-1,3)(beta-1,4)-D-Glucans, e.g. lichenan; Derivatives thereof
- C08B37/0033—Xanthan, i.e. D-glucose, D-mannose and D-glucuronic acid units, saubstituted with acetate and pyruvate, with a main chain of (beta-1,4)-D-glucose units; Derivatives thereof
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Abstract
The invention discloses a kind of preparation method and applications for thickening modified xantham gum, belong to the synthesis and technical field of modification of high molecular material, preparation comprises the steps of: that styrene-maleic anhydride copolymer, which is carried out graft esterification with xanthan gum, to react, the crude product that reaction obtains is purified, pure thickening modified xantham gum is obtained；Wherein the main chain of styrene-maleic anhydride copolymer is polystyrene, and side chain contains anhydride group；Styrene-maleic anhydride copolymer is reacted with the graft esterification of xanthan gum for homogeneous reaction.Viscosity of the thickening modified xantham gum that the present invention obtains in saline solution increases than natural viscosity of xanthan gums before modified, and has viscosity higher.
Description
Technical field
The present invention relates to a kind of preparation method and applications for thickening modified xantham gum, belong to the synthesis of high molecular material with
Technical field of modification.
Background technique
Xanthan gum is also referred to as yellow glue, xanthan gum, is microorganism using carbohydrate as the fermented engineering of primary raw material
A kind of soluble biological polyoses of production, source is unrestricted and safety is renewable.Xanthan gum is also to be most widely used at present,
The highest microbial polysaccharide of commercialization degree.Xanthan gum is a kind of heteroglycan, and primary structure includes two glucose units, two
Mannosyl units, a glucuronic acid unit, molar ratio 2.8/2.0/2.0.Xanthan gum backbone chemistry structure and cellulose
Identical, side chain terminal mannose is connected with pyruvic acid, and Molecular Weight of Xanthan Gum distribution is 2 × 106To 2 × 107Between.
Xanthan gum is because of its water solubility, tackifying, acid and alkali resistance, salt stability, excellent rheological behavior,
And the advantages such as low temperature resistant high temperature, it is widely used in the various aspects such as oil exploitation, daily-use chemical industry, food and medicine, drilling well
It is able to maintain wellbore using xanthan gum in journey to clean, the tertiary oil recovery process addition resulting crude oil of xanthan gum is higher than water drive yield, product
Matter is good.Chemicals of the crude oil industry used in oil field mainly has polyacrylamide, modified starch, hydroxylmethyl cellulose at present
Element etc., in contrast, using the relatively low of oil yield in dig a well when these substances higher cost but oil recovery process, xanthan gum exists
The performance of thickening thickening, acidproof alkali salt and anti-pollution etc. is far superior to above-mentioned substance, therefore can be in drilling fluid, completion fluid
Middle addition xanthan gum is used as tackifier.Effect of the xanthan gum in seawater, permafrost and high halogen layer ground drilling well is especially apparent,
It is especially excellent in during drilling well and tertiary oil recovery, bit speed and tar productivity have very significantly after addition xanthan gum
Raising, and blowout occurs, the probability for phenomena such as oil field collapses declines to a great extent, and oil gas field has obtained good protection.But xanthan
Viscosity of the glue in saline solution is not high, affects its application in terms of oil exploitation.
Summary of the invention
The first purpose of the invention is to provide the short thickening of a kind of simple process, mild condition, reaction time is modified
The preparation method of xanthan gum, obtained modified xantham gum have high viscosity in saline solution.
To achieve the goals above, The technical solution adopted by the invention is as follows:
A kind of preparation method thickening modified xantham gum comprising the steps of:
Styrene-maleic anhydride copolymer and xanthan gum are carried out graft esterification to react, the crude product that reaction is obtained into
Row purifying, obtains pure thickening modified xantham gum；
Wherein the main chain of styrene-maleic anhydride copolymer is polystyrene, and side chain contains anhydride group；Styrene-horse
Carry out acid anhydride copolymer to be reacted with the graft esterification of xanthan gum for homogeneous reaction；Xanthan gum solution is prepared, is selected miscible with water energy
Organic solvent dissolve styrene-maleic anhydride copolymer, the two mixing is in homogeneous.
In order to make the thickening modified xantham gum being prepared have mobility that is highly viscous while having kept, to for increasing
The content of maleic anhydride has strict requirements in the styrene-maleic anhydride copolymer of thick modified xantham gum, wherein styrene-horse
Carry out the molar ratio of maleic anhydride monomer and styrene monomer in acid anhydride copolymer and be not more than 1:10, maleic anhydride content is more than this hair
When bright range, the problem of will cause the poor fluidity because caused by increasing xanthan gum crosslinking degree.
Styrene-maleic anhydride copolymer prepared by the present invention, main chain are polystyrene, and anhydride group is connected to side chain
On, styrene-maleic anhydride copolymer is prepared by the following method: maleic anhydride, styrene and initiator are dissolved in first
In solvent, reacted at being 50~60 DEG C in bath temperature, wherein maleic anhydride and styrene are 1:10~1 in molar ratio:
30 feed intake, and remove the first solvent after reaction, and being dried to obtain main chain is the benzene that polystyrene, side chain contain anhydride group
Ethylene maleic acid anhydride copolymer；First solvent is preferably acetone, and reaction temperature controls below the boiling temperature of acetone.
Wherein, the initiator is one of azodiisobutyronitrile, azobisisoheptonitrile or dibenzoyl peroxide,
It can attempt using other azo type free radical initiators or organic peroxide evocating agent.Wherein the initiator amount accounts for
The 1%~1.2% of styrene weight.
In order to which styrene-maleic anhydride copolymer and xanthan gum more efficient can react, make styrene-maleic anhydride copolymer
Object and xanthan gum react under homogeneous system, specifically include following operation: preparing xanthan gum solution, match preparation of styrene-Malaysia
Acid anhydride copolymer acetone soln, by the acetone soln of styrene-maleic anhydride copolymer and xanthan gum solution in bath temperature
It is to be reacted at 55~65 DEG C, since acetone and water can be miscible, whole system is in homogeneous；In order to fill substrate contact more
Divide, the mobility that should have been had using the xanthan gum solution that xanthan gum is prepared, the xanthan gum solution concentration of preparation is preferably
≤ 2% (w/w).Modified xantham gum in salting liquid with high viscosity and good fluidity in order to obtain also needs strict control yellow
The material ratio of virgin rubber and styrene-maleic anhydride copolymer is by xanthan gum and styrene-maleic anhydride copolymer mass ratio
100:1~100:5 is mixed.
Select suitable second solvent to precipitate thickening modified xantham gum crude product obtained above, further with this second
Solvent washs copolymer precipitating, is dried, and pure thickening modified xantham gum is obtained.Wherein the second solvent be selected from ethyl alcohol,
At least one of isopropanol, n-butanol, dimethyl sulfoxide.
The invention also discloses mud conditioning, completion fluid and tertiary oil recovery side of the thickening modified xantham gum solution in drilling well
The application in face.
Beneficial effects of the present invention:
(1) viscosity of the thickening modified xantham gum in saline solution increases than natural viscosity of xanthan gums before modified, in salt
There is viscosity higher in aqueous solution.
(2) preparation process that the present invention designs is ingenious, reaction condition is mild, the reaction time is short, can effectively save the energy.
(3) content by control for maleic anhydride in the styrene-maleic anhydride copolymer of modified xantham gum, makes to change
Property xanthan gum have mobility that is highly viscous while having kept, prevent from causing because maleic anhydride content is bigger than normal xanthan gum to be crosslinked journey
Spend it is higher, so as to cause xanthan gum be in solid-state；When controlling the content of maleic anhydride in styrene-maleic anhydride copolymer, also answer
Guarantee that obtained phenylethylene-maleic anhydride can react under homogeneous system with xanthan gum, with the modification used in the prior art
Agent is compared with the out-phase reaction of xanthan gum, the homogeneous reaction of styrene-maleic anhydride copolymer and xanthan gum that the present invention uses,
It can significantly reduce reaction temperature, greatly shorten the reaction time.
Detailed description of the invention
The infrared spectrogram of Fig. 1 thickening modified xantham gum copolymer.
The test of modified xantham gum solution viscosity is thickened under Fig. 2 different shear rate.
Specific embodiment
Embodiment 1
Step 1: first weighing 0.98 gram of maleic anhydride and 0.104 gram of azodiisobutyronitrile, be added to containing 10.4 grams of benzene second
In the 100ml three-necked flask of alkene, then 40 milliliters of acetone are added, three-necked flask is then placed in the thermostatted water with magnetic stirring apparatus
It is reacted for 24 hours in bath at 60 DEG C, reactant is placed in draught cupboard and removes acetone solvent, then is dried under vacuum to constant weight, synthesis obtains
Main chain is the styrene-maleic anhydride copolymer that polystyrene, side chain contain anhydride group；
Step 2: 1 gram of xanthan gum being slowly added into 100 milliliters of distilled water under magnetic stirring, configures the Huang of 1wt%
Virgin rubber aqueous solution；Then the acetone soln for preparing the styrene-maleic anhydride copolymer of 1wt%, by xanthan gum solution and benzene
The acetone soln of ethylene maleic acid anhydride copolymer is 100:3 mixing by volume, under the conditions of water bath with thermostatic control is 65 DEG C, reaction 6
Hour, obtain thickening modified xantham gum crude product in solution；
Step 3: thickening modified xantham gum crude product in solution obtained above is added drop-wise in excessive alcohol solvent and is precipitated,
It is further precipitated with this copolymer of ethanol washing, is dried under vacuum to constant weight after purification, obtains pure thickening modified xantham gum, numbered
1。
Embodiment 2
Such as embodiment 1, but maleic anhydride is 0.98 gram in step 1, and styrene is 20.8 grams；Other and embodiment
As 1, thickening modified xantham gum, number 2 are obtained.
Embodiment 3
Such as embodiment 1, but maleic anhydride is 0.98 gram in step 1, and styrene is 26.0 grams, other and embodiment
As 1, thickening modified xantham gum, number 3 are obtained.
Embodiment 4
Such as embodiment 1, but maleic anhydride is 0.98 gram in step 1, and styrene is 31.2 grams, other and embodiment
As 1, thickening modified xantham gum, number 4 are obtained.
Embodiment 5
Step 1: first weighing 0.98 gram of maleic anhydride and 0.125 gram of azobisisoheptonitrile, be added to containing 10.4 grams of benzene second
In the 100ml three-necked flask of alkene, then 40 milliliters of acetone are added, three-necked flask is then placed in the thermostatted water with magnetic stirring apparatus
It is reacted for 24 hours in bath at 50 DEG C, reactant is placed in draught cupboard and removes acetone solvent, then is dried under vacuum to constant weight, synthesis obtains
Main chain is the styrene-maleic anhydride copolymer that polystyrene, side chain contain anhydride group；
Step 2: 1 gram of xanthan gum being slowly added into 100 milliliters of distilled water under magnetic stirring, configures the Huang of 1wt%
Virgin rubber aqueous solution；Then the acetone soln for preparing the styrene-maleic anhydride copolymer of 1wt%, by xanthan gum solution and benzene
The acetone soln of ethylene maleic acid anhydride copolymer is 100:1 mixing by volume, under the conditions of water bath with thermostatic control is 55 DEG C, reaction 6
Hour, obtain thickening modified xantham gum crude product in solution, number 5.
Embodiment 6
Such as embodiment 1, but maleic anhydride is 0.98 gram in step 1, and styrene is 20.8 grams, diphenyl peroxide first
0.125 gram of acyl；In step 2, the acetone soln of xanthan gum solution and styrene-maleic anhydride copolymer is by volume
100:5, other obtain thickening modified xantham gum, number 6 in the same manner as in Example 1.
The synthesizing formula of the thickening modified xantham gum of table 1
A) A, B, C, D represent maleic anhydride-styrene copolymers sample, wherein mole score of maleic anhydride and styrene
Wei 1:10,1:20,1:25 or 1:30.b): initiator is azodiisobutyronitrile when synthesis of maleic anhydride-styrol copolymer,
C): initiator is azobisisoheptonitrile, d when synthesis of maleic anhydride-styrol copolymer): synthesis of maleic anhydride-
Initiator is dibenzoyl peroxide when styrol copolymer.
Embodiment 7
The structure of thickening modified xantham gum is analyzed using Fourier's Total Reflection Infrared instrument: grinding sample, opens instrument
With computer, it is arranged after adjusting parameter and wipes detection mouth with alcohol swab, a small amount of sample is taken to be placed on infrared spectrograph sample platform,
4000cm-1~400cm-1Scanning, obtains its infrared spectrogram (Fig. 1) in range.Thicken the infrared spectroscopy diagram of modified xantham gum
Analysis: 3300-1Cm or so appearance is the peak value that O-H stretching vibration generates；2900-1The possibility that cm or so occurs is stretched for C-H
The peak value that contracting vibration generates；1600-1Cm or so appearance is the skeletal vibration of substituted benzene, illustrates success on modified xantham gum
Introduce styrene；1400-1The peak value that cm or so occurs is the C-H in-plane bending vibration of olefines；1240-1Cm is left
The peak value of right appearance is C-O stretching vibration；1030-1The peak value that cm or so occurs is O-H out-of-plane bending vibration；700-1cm
The peak value that left and right occurs is the C-H out-of-plane bending vibration on phenyl ring.By above peakology can obtain copolymer with xanthan
The conclusion of glue reaction, i.e. xanthan gum have been copolymerized object and have been modified, and have obtained mesh target product.
Embodiment 8
Viscosity test under different temperatures: the saline solution that NaCl concentration is 0.28wt% is prepared, then by number is 1,2,3,4
Thickening modified xantham gum sample solution be added separately to above-mentioned saline solution, make sample concentration 0.5wt%, be respectively placed in and shake
Then constant temperature 4h in bed chooses S05 type rotor, rotated with the speed of shear rate 12 (r/min).At different temperatures (20 DEG C,
30 DEG C, 40 DEG C) measurement viscosity, the viscosimetric analysis of each sample 3 times, final result takes 3 average value, and the results are shown in Table 2.
The result shows that: the viscosity of thickening modified xantham gum sample is higher than the viscosity of xanthan gum before modified.
The viscosity (mpa.s) of modified xantham gum is thickened under 2 different temperatures of table
Embodiment 9
Viscosity test under different shear rate: preparing the saline solution that NaCl concentration is 0.28wt%, then by number be 1,
2,3,4 thickening modified xantham gum sample solution is added separately to above-mentioned saline solution, makes sample concentration 1wt%, sets respectively
Then 20 DEG C of 4h of constant temperature in shaking table choose S05 type rotor, viscosity, the viscosity of each sample are measured under different shear rate
Measurement 3 times, final result takes 3 average value results as shown in Figure 2.The result shows that: as shear rate increases, under viscosity
Drop.
Claims (10)
1. a kind of preparation method for thickening modified xantham gum, which is characterized in that comprise the steps of:
Styrene-maleic anhydride copolymer is carried out graft esterification with xanthan gum to react, the crude product that reaction is obtained carries out pure
Change, obtains pure thickening modified xantham gum；
Wherein the main chain of styrene-maleic anhydride copolymer is polystyrene, and side chain contains anhydride group；Styrene-maleic acid
Anhydride copolymer is reacted with the graft esterification of xanthan gum for homogeneous reaction.
2. the preparation method of thickening modified xantham gum according to claim 1, it is characterised in that: phenylethylene-maleic anhydride
The molar ratio of maleic anhydride monomer and styrene monomer is not more than 1:10 in copolymer.
3. the preparation method of thickening modified xantham gum according to claim 1, it is characterised in that: phenylethylene-maleic anhydride
Copolymer is prepared by the following method: maleic anhydride, styrene and initiator being dissolved in the first solvent, in bath temperature
It is to be reacted at 50 ~ 60 DEG C, wherein maleic anhydride and styrene are that 1:10 ~ 1:30 feeds intake in molar ratio, and reaction terminates
After remove the first solvent, being dried to obtain main chain is the styrene-maleic anhydride copolymer that polystyrene, side chain contain anhydride group
Object.
4. the preparation method of thickening modified xantham gum according to claim 3, it is characterised in that: first solvent is third
The preparation of ketone, styrene-maleic anhydride copolymer carries out below acetone boiling temperature.
5. the preparation method of thickening modified xantham gum according to claim 3, it is characterised in that: maleic anhydride and styrene
It feeds intake in molar ratio for 1:20 ~ 1:26, the initiator is azodiisobutyronitrile, azobisisoheptonitrile or diphenyl peroxide
One of formyl.
6. the preparation method of thickening modified xantham gum according to claim 1, it is characterised in that: phenylethylene-maleic anhydride
Copolymer is reacted with the graft esterification of xanthan gum to be comprised the steps of: preparation xanthan gum solution, prepares phenylethylene-maleic anhydride
Copolymer acetone soln, by the acetone soln of styrene-maleic anhydride copolymer and xanthan gum solution by xanthan gum and benzene second
Alkene-copolymer-maleic anhydride mass ratio is that 100:1 ~ 100:5 carries out hybrid reaction.
7. the preparation method of thickening modified xantham gum according to claim 6, it is characterised in that: the xanthan gum solution
Concentration≤2%(w/w), styrene-maleic anhydride copolymer reacted with the graft esterification of xanthan gum bath temperature be 55 ~ 65
It is carried out at DEG C.
8. the preparation method of thickening modified xantham gum according to claim 7, it is characterised in that: phenylethylene-maleic anhydride
The reaction time that copolymer is reacted with the graft esterification of xanthan gum is 4 ~ 6h.
9. the preparation method of thickening modified xantham gum according to claim 1, it is characterised in that: the thick production for obtaining reaction
Object precipitated with the second solvent, is washed with second solvent, is dried to precipitating again, and the modified xanthan of pure thickening is obtained
Glue, wherein the second solvent is at least one of ethyl alcohol, isopropanol, n-butanol, dimethyl sulfoxide.
10. what the preparation method for thickening modified xantham gum described in any claim according to claim 1 ~ 9 was prepared changes
Application in terms of mud conditioning, completion fluid and tertiary oil recovery of the property xanthan gum in drilling process.
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| CN110642961A (en) * | 2019-11-14 | 2020-01-03 | 刘建阳 | Preparation method of hydrophobically modified xanthan gum |
| CN112480285A (en) * | 2020-11-16 | 2021-03-12 | 山东省食品发酵工业研究设计院 | Method for preparing calcium ion resistant xanthan gum through chemical modification |
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