CN104151442A - Surface hydrophobic modified xanthan gum and preparation method thereof - Google Patents
Surface hydrophobic modified xanthan gum and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a surface hydrophobic modified xanthan gum which is prepared from the following steps: (1) 2-6 parts by weight of calcium chloride, 4-8 parts by weight of iron trichloride, 1-6 parts by weight of sodium metaaluminate, 5-15 parts by weight of hydrochloric acid (36%), 3.5-5.5 parts by weight of sodium polyacrylate and 5-30 parts by weight of distilled water are fully stirred and mixed to obtain a liquid reactant A; (2) the xanthan gum is stirred and mixed with ethanol and toluene with the mass ratio of 0.5:1 to 4:1 and 0.1:1 to 1.5: 1 for 30 min to obtain a xanthan gum dispersing system, wherein the mass ratio of the ethanol to the xanthan gum is (0.5:1)-(4:1), and the mass ratio of the toluene to the xanthan gum is (0.1:1)-(1.5:1); (3) the liquid reactant A is added to the xanthan gum dispersing system and stirred at constant temperature of 30-60 DEG C for 2 h, wherein the mass ratio of the xanthan gum to the liquid reactant A is (1:1)-(1: 4); (4) then, bromo-alkane is slowly added into the mixture dropwise to be continuously stirred at constant temperature for 4 h, wherein the mass ratio of the xanthan gum to the bromo-alkane is (10:1)-(100:1); (5) the solution prepared in the step (4) is subjected to suction filtration and dried at the temperature of 70-90 DEG C for 4 h to obtain the surface hydrophobic modified xanthan gum.
Description
Technical field
The present invention relates to xanthan gum of a kind of surface hydrophobicity modification and preparation method thereof.
Background technology
Xanthan gum is a kind of conventional drilling fluid flow pattern regulator, has tackify and proposes the effect of cutting.Add in drilling fluid, can significantly improve viscosity and the shear force of drilling fluid.
Add to drilling fluid in the process of xanthan gum, due to the viscosifying action of xanthan gum, the xanthan gum molecule first contacting with water can rapid aquation and is formed the hydration layer of one deck densification, and obstruction water molecules is to the internal divergence of xanthan gum particle.In the time that agitation condition is bad, just can form agglomerate.Drilling practice shows, even if through the high speed shear of bit port, still has a large amount of xanthan gum cannot dispersing and dissolving.Arrive after vibratory screening apparatus, just can be removed by Vibration Screen, cause very large waste.
For addressing the above problem, situ of drilling well is generally joined mud shearing pump, is improved the engineering measures such as stirring rake speed by increasing.But above method practical effect is not good.In addition, some xanthan gum manufacturers pass through to improve the zymotechnique of xanthan gum, thereby have improved the dissolution rate of xanthan gum, but cannot change the dispersing property of xanthan gum, therefore cannot solve the agglomerate problem producing in xanthan gum process for preparation at all.
Thereby, exist thering is the demand of xanthan gum of surface hydrophobicity modification and preparation method thereof.
Summary of the invention
An object of the present invention is to provide a kind of xanthan gum of surface hydrophobicity modification.
Another object of the present invention is to provide a kind of method of the xanthan gum of preparing surperficial hydrophobically modified.
The xanthan gum of surface hydrophobicity modification of the present invention is prepared by following steps:
(1) hydrochloric acid (36%) of the sodium metaaluminate of the iron trichloride of the calcium chloride of 2 to 6 weight parts, 4 to 8 weight parts, 1 to 6 weight part, 5 to 15 weight parts, the sodium polyacrylate of 3.5 to 5.5 weight parts and the distilled water of 5 to 30 weight parts are fully uniformly mixed, obtain reaction solution A;
(2) be uniformly mixed 30min and obtain xanthan gum dispersion system being respectively the ethanol of 0.5:1 to 4:1 and 0.1:1 to 1.5:1 and toluene with xanthan gum mass ratio;
(3) described reaction solution A is joined in described xanthan gum dispersion system, and the mass ratio of xanthan gum and described reaction solution A is 1:1 to 1:4, then at 30 DEG C～60 DEG C, constant temperature stirs 2h;
(4) then slowly drip brominated alkanes, and the mass ratio of xanthan gum and brominated alkanes is 10:1 to 100:1, continues constant temperature and stir 4h;
(5) solution of step 4 gained is carried out to suction filtration, and dry 4h at 70 DEG C～90 DEG C, obtain the xanthan gum of surface hydrophobicity modification.
Preferably, the molecular weight of sodium polyacrylate is 1000～5000.
Preferably, brominated alkanes is that carbon number is a bromo straight-chain paraffin of 8-16.
The method of the xanthan gum of the surperficial hydrophobically modified of preparation of the present invention comprises the following steps:
(1) hydrochloric acid (36%) of the sodium metaaluminate of the iron trichloride of the calcium chloride of 2 to 6 weight parts, 4 to 8 weight parts, 1 to 6 weight part, 5 to 15 weight parts, the sodium polyacrylate of 3.5 to 5.5 weight parts and the distilled water of 5 to 30 weight parts are fully uniformly mixed, obtain reaction solution A;
(2) be uniformly mixed 30min and obtain xanthan gum dispersion system being respectively the ethanol of 0.5:1 to 4:1 and 0.1:1 to 1.5:1 and toluene with xanthan gum mass ratio;
(3) described reaction solution A is joined in described xanthan gum dispersion system, and the mass ratio of xanthan gum and described reaction solution A is 1:1 to 1:4, then at 30 DEG C～60 DEG C, constant temperature stirs 2h;
(4) then slowly drip brominated alkanes, and the mass ratio of xanthan gum and brominated alkanes is 10:1 to 100:1, continues constant temperature and stir 4h;
(5) solution of step 4 gained is carried out to suction filtration, and dry 4h at 70 DEG C～90 DEG C, obtain the xanthan gum of surface hydrophobicity modification.
The present invention has solved agglomeration problems effectively by xanthan gum particle surface is carried out to hydrophobically modified.The xanthan gum of surface hydrophobicity modification of the present invention after being added to the water, not aquation immediately, but be scattered in equably in water, then homodisperse xanthan gum particle is under water diffusion effect, aquation tackify gradually, until aquation is dissolved completely, thereby can not produce agglomerate.
The dissolution time of the xanthan gum of surface hydrophobicity modification of the present invention is greater than 85%, produces without agglomerate in dissolution process lower than 60min, dissolution rate.
Compared with prior art, the present invention has following beneficial effect:
(1) xanthan gum of surface hydrophobicity modification of the present invention can be disperseed rapidly in drilling fluid, even if stir under bad condition, still good dispersion, does not produce agglomerate, has solved the problem of xanthan gum generation agglomerate in drilling fluid process for preparation;
(2), compared with unmodified xanthan gum, the xanthan gum dissolution time of surface hydrophobicity modification of the present invention is shorter, dissolution rate is higher;
(3) compared with being not less than the unmodified xanthan gum under equal conditions with final viscosity, the xanthan gum of surface hydrophobicity modification of the present invention is not in reducing xanthan gum Efficient Adhesive Promotion, improve significantly the dissolution rate of xanthan gum, reduced the service wear of xanthan gum.
Embodiment
Xanthan gum in embodiments of the invention can adopt the drilling well level xanthan gum that meets " API RP 13A:Specification for Drilling Fluids Materials " standard-required, for ensureing experiment unity, the xanthan gum product that the xanthan gum of following embodiment all adopts Neimenggu Fufeng Biotechnologies Co., Ltd to produce.
Embodiment 1
Take 40.00g toluene and 15.00g ethanol, be transferred in there-necked flask; Take 10.00g xanthan gum, join in there-necked flask, open and stir simultaneously, continue to stir 30min; Take 2.00g calcium chloride, 5.00g iron trichloride, 2.00g sodium metaaluminate, 7.00g concentrated hydrochloric acid (36%) and 4.00g sodium polyacrylate, join in 20.00g distilled water and fully dissolve, then solution is joined in there-necked flask; Open heating in water bath, at 50 DEG C, constant temperature stirs 2h; Take 1.00g bromodecane, slowly drop in there-necked flask, at 50 DEG C, continue constant temperature and stir 4h; Reaction finishes, and takes out reaction solution and carries out suction filtration, at 80 DEG C, dries 4h; After oven dry, obtain micro-yellow free-flowing powder powder sample, be the xanthan gum of surface hydrophobicity modification.
Performance test:
(1) in 980.00g deionized water, add 41.95g sea salt, preparation manually substitutes seawater;
(2) take the above-mentioned seawater 412.00g that manually substitutes, be transferred in the measuring cup of rotational viscosimeter;
(3) rotating speed of rotational viscosimeter is adjusted to 600 revs/min;
(4) whether xanthan gum (or the raw material xanthan gum) 2.00g that takes prepared surface hydrophobicity modification, as testing sample and joining fast in the measuring cup of rotational viscosimeter, has agglomerate to produce in observation.
(5) after test sample adds, read the apparent viscosity of a sample every 1min, record sample viscosity rule over time.In the time that the increased value of sample viscosity in 10min is less than 0.5mPas, record is time and the sample apparent viscosity of correspondence now.Apparent viscosity is now designated as dissolving viscosity, and institute is designated as dissolution time the corresponding time.
(6) by above-mentioned test sample, be transferred in sealed vessel.Place after 6h, on rotational viscosimeter, measure the apparent viscosity under 600rpm, be designated as sample final viscosity.
(7) dissolution degree of sample can represent with dissolution rate, and the larger expression sample dissolution of dissolution rate more abundant represents that in the time that dissolution rate is 100% sample dissolves completely.Dissolution rate is calculated as follows:
Dissolution rate=dissolving viscosity/final viscosity × 100%
After tested, after the sample dissolution of the present embodiment gained, without agglomerate, its property indices is as follows:
| Sample title | Dissolution time, min | Dissolution rate, % | Final viscosity, mPas |
| The sample of embodiment 1 | 54 | 86 | 17.5 |
| Raw material xanthan gum | 75 | 82 | 17 |
Embodiment 2
Take 25.00g toluene and 25.00g ethanol, be transferred in there-necked flask; Take 25.00g xanthan gum, join in there-necked flask, open and stir simultaneously, continue to stir 30min; Take 5.50g calcium chloride, 8.00g iron trichloride, 1.00g sodium metaaluminate, 5.00g concentrated hydrochloric acid (36%) and 3.50g sodium polyacrylate, join in 30.00g distilled water and fully dissolve, then solution is joined in there-necked flask; Open heating in water bath, at 30 DEG C, constant temperature stirs 2h; Take 2.00g bromooctane, slowly drop in there-necked flask, at 30 DEG C, continue constant temperature and stir 4h; Reaction finishes, and takes out reaction solution and carries out suction filtration, at 90 DEG C, dries 4h; After oven dry, obtain micro-yellow free-flowing powder powder sample, be the xanthan gum of surface hydrophobicity modification.
Performance test methods according to embodiment 1 is tested, and after the sample dissolution of the present embodiment gained, without agglomerate, its property indices is as follows:
| Sample title | Dissolution time, min | Dissolution rate, % | Final viscosity, mPas |
| The sample of embodiment 2 | 45 | 90 | 18.5 |
| Raw material xanthan gum | 75 | 82 | 17 |
Embodiment 3
Take 20.00g toluene and 4.00g ethanol, be transferred in there-necked flask; Take 40.00g xanthan gum, join in there-necked flask, open and stir simultaneously, continue to stir 30min; Take 6.00g calcium chloride, 4.00g iron trichloride, 6.00g sodium metaaluminate, 15.00g concentrated hydrochloric acid (36%) and 4.00g sodium polyacrylate, join in 5.00g distilled water and fully dissolve, then solution is joined in there-necked flask; Open heating in water bath, at 60 DEG C, constant temperature stirs 2h; Take 0.40g bromododecane, slowly drop in there-necked flask, at 60 DEG C, continue constant temperature and stir 4h; Reaction finishes, and takes out reaction solution and carries out suction filtration, at 70 DEG C, dries 4h; After oven dry, obtain micro-yellow free-flowing powder powder sample, be the xanthan gum of surface hydrophobicity modification.
Performance test methods according to embodiment 1 is tested, and after the sample dissolution of the present embodiment gained, without agglomerate, its property indices is as follows:
| Sample title | Dissolution time, min | Dissolution rate, % | Final viscosity, mPas |
| The sample of embodiment 3 | 36 | 92 | 21 |
| Raw material xanthan gum | 75 | 82 | 17 |
Embodiment 4
Take 30.00g toluene and 18.00g ethanol, be transferred in there-necked flask; Take 15.00g xanthan gum, join in there-necked flask, open and stir simultaneously, continue to stir 30min; Take 4.50g calcium chloride, 4.50g iron trichloride, 2.50g sodium metaaluminate, 7.00g concentrated hydrochloric acid (36%) and 5.50g sodium polyacrylate, join in 15.00g distilled water and fully dissolve, then solution is joined in there-necked flask; Open heating in water bath, at 40 DEG C, constant temperature stirs 2h; Take 0.30g bromotetradecane, slowly drop in there-necked flask, at 40 DEG C, continue constant temperature and stir 4h; Reaction finishes, and takes out reaction solution and carries out suction filtration, at 80 DEG C, dries 4h; After oven dry, obtain micro-yellow free-flowing powder powder sample, be the xanthan gum of surface hydrophobicity modification.
Performance test methods according to embodiment 1 is tested, and after the sample dissolution of the present embodiment gained, without agglomerate, its property indices is as follows:
| Sample title | Dissolution time, min | Dissolution rate, % | Final viscosity, mPas |
| The sample of embodiment 4 | 48 | 94 | 21.5 |
| Raw material xanthan gum | 75 | 82 | 17 |
Embodiment 5
Take 75.00g toluene and 15.00g ethanol, be transferred in there-necked flask; Take 25.00g xanthan gum, join in there-necked flask, open and stir simultaneously, continue to stir 30min; Take 2.50g calcium chloride, 7.00g iron trichloride, 4.50g sodium metaaluminate, 10.00g concentrated hydrochloric acid (36%) and 4.50g sodium polyacrylate, join in 10.00g distilled water and fully dissolve, then solution is joined in there-necked flask; Open heating in water bath, at 50 DEG C, constant temperature stirs 2h; Take 0.33g bromohexadecane, slowly drop in there-necked flask, at 50 DEG C, continue constant temperature and stir 4h; Reaction finishes, and takes out reaction solution and carries out suction filtration, at 80 DEG C, dries 4h; After oven dry, obtain micro-yellow free-flowing powder powder sample, be the xanthan gum of surface hydrophobicity modification.
Performance test methods according to embodiment 1 is tested, and after the sample dissolution of the present embodiment gained, without agglomerate, its property indices is as follows:
| Sample title | Dissolution time, min | Dissolution rate, % | Final viscosity, mPas |
| The sample of embodiment 5 | 38 | 96 | 22 |
| Raw material xanthan gum | 75 | 82 | 17 |
Judgement criteria:
Add after the xanthan gum of surface hydrophobicity modification should produce without agglomerate, dissolution time is shorter, dissolution rate is higher, final viscosity is not less than the raw material xanthan gum under equal conditions.
From the performance test results of embodiment 1～embodiment 5, after the surface of xanthan gum particle is hydrophobically modified, its dispersiveness is improved greatly, even if (rotating speed 600rpm is equivalent to shearing rate 1022s at low velocity shear
-1) under, still produce without agglomerate.And from unmodified xanthan gum, the scene of raw material xanthan gum makes for seeing, even if the shearing rate at bit port place is at 10000s
-1above, still have a large amount of agglomerates to produce.Due to the improvement of dispersing property, after surface hydrophobicity modification xanthan gum is dispersed in water, its specific surface area increases, and the chance contacting with water increases, thereby dissolution time shortens, dissolution rate improves, and final viscosity is suitable with raw material xanthan gum.
Although the disclosed embodiment of the application as above, the embodiment that described content just adopts for the ease of understanding the application, not in order to limit the application.Technician under any the application in technical field; do not departing under the prerequisite of the disclosed spirit and scope of the application; can do any amendment and variation what implement in form and in details; but the application's protection domain, still must be as the criterion with the scope that appending claims was defined.
Claims (6)
1. an xanthan gum for surface hydrophobicity modification, it is prepared by following steps:
(1) hydrochloric acid (36%) of the sodium metaaluminate of the iron trichloride of the calcium chloride of 2 to 6 weight parts, 4 to 8 weight parts, 1 to 6 weight part, 5 to 15 weight parts, the sodium polyacrylate of 3.5 to 5.5 weight parts and the distilled water of 5 to 30 weight parts are fully uniformly mixed, obtain reaction solution A;
(2) be uniformly mixed 30min and obtain xanthan gum dispersion system being respectively the ethanol of 0.5:1 to 4:1 and 0.1:1 to 1.5:1 and toluene with xanthan gum mass ratio;
(3) described reaction solution A is joined in described xanthan gum dispersion system, and the mass ratio of xanthan gum and described reaction solution A is 1:1 to 1:4, then at 30 DEG C～60 DEG C, constant temperature stirs 2h;
(4) then slowly drip brominated alkanes, and the mass ratio of xanthan gum and brominated alkanes is 10:1 to 100:1, continues constant temperature and stir 4h;
(5) solution of step 4 gained is carried out to suction filtration, and dry 4h at 70 DEG C～90 DEG C, obtain the xanthan gum of surface hydrophobicity modification.
2. the xanthan gum of surface hydrophobicity modification according to claim 1, is characterized in that: the weight-average molecular weight of sodium polyacrylate is 1000～5000.
3. the xanthan gum of surface hydrophobicity modification according to claim 1, is characterized in that: described brominated alkanes is that carbon number is a bromo straight-chain paraffin of 8-16.
4. a method of preparing the xanthan gum of surperficial hydrophobically modified, it comprises the following steps:
(1) hydrochloric acid (36%) of the sodium metaaluminate of the iron trichloride of the calcium chloride of 2 to 6 weight parts, 4 to 8 weight parts, 1 to 6 weight part, 5 to 15 weight parts, the sodium polyacrylate of 3.5 to 5.5 weight parts and the distilled water of 5 to 30 weight parts are fully uniformly mixed, obtain reaction solution A;
(2) be uniformly mixed 30min and obtain xanthan gum dispersion system being respectively the ethanol of 0.5:1 to 4:1 and 0.1:1 to 1.5:1 and toluene with xanthan gum mass ratio;
(3) described reaction solution A is joined in described xanthan gum dispersion system, and the mass ratio of xanthan gum and described reaction solution A is 1:1 to 1:4, then at 30 DEG C～60 DEG C, constant temperature stirs 2h;
(4) then slowly drip brominated alkanes, and the mass ratio of xanthan gum and brominated alkanes is 10:1 to 100:1, continues constant temperature and stir 4h;
(5) solution of step 4 gained is carried out to suction filtration, and dry 4h at 70 DEG C～90 DEG C, obtain the xanthan gum of surface hydrophobicity modification.
5. method according to claim 4, is characterized in that: the molecular weight weight-average molecular weight of sodium polyacrylate is 1000～5000.
6. method according to claim 4, is characterized in that: described brominated alkanes is that carbon number is a bromo straight-chain paraffin of 8-16.
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| CN201410378538.6A CN104151442B (en) | 2014-08-01 | 2014-08-01 | Xanthan gum of a kind of surface hydrophobicity modification and preparation method thereof |
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| CN201410378538.6A CN104151442B (en) | 2014-08-01 | 2014-08-01 | Xanthan gum of a kind of surface hydrophobicity modification and preparation method thereof |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106699414A (en) * | 2017-02-17 | 2017-05-24 | 衡水东辉生物科技有限公司 | Fertilizer additive and preparation method and use thereof |
| CN110235935A (en) * | 2019-05-22 | 2019-09-17 | 重庆市林业科学研究院 | A kind of fresh bamboo shoot antistaling agent and preparation method and application |
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| CN103724443A (en) * | 2013-12-17 | 2014-04-16 | 山东大学 | Method for preparing hydrophobically modified xanthan |
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103724443A (en) * | 2013-12-17 | 2014-04-16 | 山东大学 | Method for preparing hydrophobically modified xanthan |
Non-Patent Citations (1)
| Title |
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| 钱晓琳等: "疏水改性黄原胶HMXG—C8水溶液黏度特征", 《油田化学》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106699414A (en) * | 2017-02-17 | 2017-05-24 | 衡水东辉生物科技有限公司 | Fertilizer additive and preparation method and use thereof |
| CN110235935A (en) * | 2019-05-22 | 2019-09-17 | 重庆市林业科学研究院 | A kind of fresh bamboo shoot antistaling agent and preparation method and application |
| CN110235935B (en) * | 2019-05-22 | 2022-04-29 | 重庆市林业科学研究院 | Fresh bamboo shoot preservative and preparation method and application thereof |
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Address after: 100010 Chaoyangmen North Street, Dongcheng District, Dongcheng District, Beijing Co-patentee after: China Oilfield Services Limited Patentee after: China Offshore Oil Group Co., Ltd. Address before: 100010 Chaoyangmen North Street, Dongcheng District, Dongcheng District, Beijing Co-patentee before: China Oilfield Services Limited Patentee before: China National Offshore Oil Corporation |
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