CN104558235A - Preparation method of high-viscosity modified guar gum - Google Patents
Preparation method of high-viscosity modified guar gum Download PDFInfo
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- CN104558235A CN104558235A CN201510040786.4A CN201510040786A CN104558235A CN 104558235 A CN104558235 A CN 104558235A CN 201510040786 A CN201510040786 A CN 201510040786A CN 104558235 A CN104558235 A CN 104558235A
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- guar gum
- modified guar
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Abstract
The invention discloses a preparation method of a high-viscosity modified guar gum. The preparation method is characterized by comprising the following steps: adding sheeted guar gum, a liquid alkali, an etherifying agent, carbon dioxide and water into a high-pressure resistant reactor, carrying out alkalization reaction and etherification reaction at a temperature in sections to obtain an modified guar gum, washing and centrifuging the modified guar gum to obtain a purified product, super-grinding the purified product, drying a high speed, micro-grinding under the vortex of airflow, and separating to obtain the finished product which is the high-viscosity modified guar gum. The continuously mixed high-viscosity modified guar gum disclosed by the invention is a white or off-white powder, has the advantages of small particle size and high swelling rate, contains less than 3% of water insoluble matters and has the viscosity of 6,200-7,500mPa.s. In addition, 100% of the high-viscosity modified guar gum can pass a 200-mesh sieve, and 98% of the high-viscosity modified guar gum can pass a 300-mesh sieve.
Description
Technical field
The present invention relates to a kind of manufacture method of high adhered modification guar gum.
Background technology
Guar gum and derivative thereof are as the of the fracturing fluid viscosifying agent of oil reservoir, for can pressure break success, increase production and improve productivity and play a key effect, most of China oil field all can use the oil field fracturing fluid of different performance, in the prior art, obtain modified guar product by carrying out modification to the hydrophilic group of guar gum molecule, in many areas, during this viscosifying agent guar products mixture, there is following defect:
1, the swelling rate in water is slow, just can reach peak viscosity for a long time;
2, use the organic solvent pollution environment in isolation technique, quantity discharged is large;
3, guar splits time in modified-reaction process is long, and reduce guar gum molecular weight, viscosity utilization ratio is low.
Summary of the invention
In order to solve the above-mentioned technical problem that guar products exists in production technique, the invention provides a kind of manufacture method of high adhered modification guar gum.The high adhered modification guar products produced by this manufacture method solves the shortcoming that guar gum viscosity is inadequate, water-insoluble is high.
The technical solution adopted for the present invention to solve the technical problems is: the manufacture method of inventing a kind of high adhered modification guar gum, it is characterized in that adding in high pressure resistant reactor that guar splits carries out quaternization, after etherification reaction obtains modified guar sheet, carry out washing centrifugal treating and obtain purified product, then by superfinishing technology, rapidly acting dry technology, air-flow vortex micro mist pulverizes and sorting technology obtains high adhered modification guar gum flour finished product;
The first step quaternization: add guar splits in high pressure resistant reactor after, under enclosed space, temperature remains on 50-60 DEG C, under the nitrogen protection of 0.03-0.06 MPa, adds liquid base, Stirring 20 ~ 30 minutes;
Second step etherification reaction: airtight vacuum pressure, temperature keeps 50 ~ 70 DEG C, under 0.01 ~ 0.03 MPa nitrogen protection, adds etherifying agent, reacts 0.5 ~ 3 hour;
3rd step: airtight vacuum pressure, adds carbon dioxide, stirs 15 minutes;
4th step: add tap water and continue stirring after 30 minutes, blowing obtains modified guar sheet, then add washing water washing centrifugal treating and obtain purified product.
In the present invention, shared by each raw material, parts by weight are as follows:
Guar splits: 300-400 part
Liquid base: 30-70 part
Etherifying agent: 60-80 part
Carbonic acid gas: 6-10 part
Tap water: 100-150 part
Washing water: 3500-4000 part
Liquid base used is 30% alkali lye, etherifying agent is propylene oxide, superfinishing technology refers to high pressure three roller grinding technique, rapidly acting dry technology refers to modified guar meal by high efficiency drying flashing apparatus, making modified guar meal reach water content is 7% ~ 10%, air-flow vortex micro mist crushing technology refers to and modified guar meal is carried out in air-flow vortex ultra-fine micropowder equipment fine powder is broken, screening, modified guar powder more than 200 orders that finally obtain sieving.
Compared with prior art, the invention has the beneficial effects as follows:
The continuous mixture high adhered modification guar gum finished product of gained of the present invention is white powder or off-white powder.Have the advantage that particle is thin, swelling rate fast, water insoluble matter content is less than 3%, 200 eye mesh screen percent of pass are 100%, 300 eye mesh screen percent of pass is 98%, and viscosity can reach 6200 ~ 7500mPa.s; Raw material involved in preparation feedback process, operational path all meet the requirement of Green Chemistry, can not produce pollutent, economy, environmental protection, strong adaptability.
Embodiment
Embodiment 1
High adhered modification guar gum production method is as follows:
Quaternization: after high pressure resistant reactor adds 300 parts of films, about keeping temperature 50 C, adds 30 parts of liquid base solution, Stirring 20 minutes under having 0.03MPa nitrogen protection;
Etherification reaction: airtight vacuum lays down pressure, temperature keeps 60 DEG C, and adds 60 portions of etherifying agents under having 0.01 MPa nitrogen protection, reacts 1 hour;
Then 6 parts of carbonic acid gas are added, stir after 15 minutes, add 100 parts of tap water and continue stirring 30 minutes, namely blowing obtains modified guar sheet, purified product is obtained after modified guar sheet being added 3500 parts of washing water washing centrifugal treating, again purified product is carried out superfinishing, highly effective drying, the process of air-flow vortex micro mist, vibratory screening apparatus screening, finally obtains the product of following performance index:
1) apparent viscosity: 7150mPa.s
2) water-insoluble: 2.5%
3) sieving rate: 100% by 200 orders, and 98% by 300 orders;
Embodiment 2
Quaternization: after high pressure resistant reactor adds 350 parts of films, temperature be 55 DEG C, Stirring 25 minutes under the condition of nitrogen pressure 0.04 MPa;
Etherification reaction: airtight vacuum lays down pressure, temperature keeps 65 DEG C, and adds 70 portions of etherifying agents under having 0.02 MPa nitrogen protection, reacts 1.5 hours;
Then 7 parts of carbonic acid gas are added, stir after 15 minutes, add 120 parts of tap water and continue stirring 30 minutes, namely blowing obtains modified guar sheet, purified product is obtained after modified guar sheet being added 3800 parts of washing water washing centrifugal treating, after this production technique is identical with embodiment 1, repeats no more, and finally obtains with the product of descending performance index:
1) apparent viscosity: 7450mPa.s
2) water-insoluble: 2.0%
3) sieving rate: 100% by 200 orders, and 98% by 300 orders;
Embodiment 3
Quaternization: after high pressure resistant reactor adds 400 parts of films, is 60 DEG C in temperature, under the condition of nitrogen pressure 0.05 MPa, adds 70 parts of liquid base solution, Stirring 30 minutes;
Etherification reaction: closed reactor vacuumizes, temperature keeps 70 DEG C, and adds 80 portions of etherifying agents under having 0.03 MPa nitrogen protection, reacts 2 hours;
Then 10 parts of carbonic acid gas are added, stir after 15 minutes, add 150 parts of tap water and continue stirring 30 minutes, namely blowing obtains modified guar sheet, purified product is obtained after modified guar sheet being added 4000 parts of washing water washing centrifugal treating, after this production technique is identical with embodiment 1, repeats no more, and finally obtains the product of following performance index:
1) apparent viscosity: 7200mPa.s
2) water-insoluble: 2.2%
3) sieving rate: 100% by 200 orders, and 98% by 300 orders
* illustrate: in the present invention, tap water used and washing water essence are all tap water, because component added in various processes step is different with order, so play different names to show difference.
The above is only preferred embodiment of the present invention, and be not restriction the present invention being made to other form, any those skilled in the art may utilize the technology contents of above-mentioned announcement to be changed or be modified as the Equivalent embodiments of equivalent variations.But everyly do not depart from technical solution of the present invention content, any simple modification, equivalent variations and the remodeling done above embodiment according to technical spirit of the present invention, still belong to the protection domain of technical solution of the present invention.
Claims (6)
1. the manufacture method of a high adhered modification guar gum, it is characterized in that adding in high pressure resistant reactor that guar splits carries out quaternization, after etherification reaction obtains modified guar sheet, carry out washing centrifugal treating and obtain purified product, then by superfinishing technology, rapidly acting dry technology, air-flow vortex micro mist pulverizes and sorting technology obtains high adhered modification guar gum flour finished product;
The first step quaternization: add guar splits in high pressure resistant reactor after, under enclosed space, temperature remains on 50-60 DEG C, under the nitrogen protection of 0.03-0.06 MPa, adds liquid base, Stirring 20 ~ 30 minutes;
Second step etherification reaction: airtight vacuum pressure, temperature keeps 50 ~ 70 DEG C, under 0.01 ~ 0.03 MPa nitrogen protection, adds etherifying agent, reacts 0.5 ~ 3 hour;
3rd step: airtight vacuum pressure, adds carbon dioxide, stirs 15 minutes;
4th step: add tap water and continue stirring after 30 minutes, blowing obtains modified guar sheet, then add washing water washing centrifugal treating and obtain purified product.
2. the manufacture method of a kind of high adhered modification guar gum according to claim 1, is characterized in that each raw material weight number is as follows:
Guar splits: 300-400 part
Liquid base: 30-70 part
Etherifying agent: 60-80 part
Carbonic acid gas: 6-10 part
Tap water: 100-150 part
Washing water: 3500-4000 part.
3. the manufacture method of a kind of high adhered modification guar gum according to claim 1 and 2, it is characterized in that described liquid base is 30% alkali lye, described etherifying agent is propylene oxide.
4. the manufacture method of a kind of high adhered modification guar gum according to claim 1, is characterized in that superfinishing technology refers to high pressure three roller grinding technique.
5. the manufacture method of a kind of high adhered modification guar gum according to claim 1, is characterized in that rapidly acting dry technology to refer to modified guar meal by high efficiency drying flashing apparatus, makes modified guar meal water content reach 7% ~ 10%.
6. the manufacture method of a kind of high adhered modification guar gum according to claim 1, it is characterized in that air-flow vortex micro mist crushing technology refers to and modified guar meal carried out in air-flow vortex ultra-fine micropowder equipment fine powder is broken, screening, modified guar powder more than 200 orders that finally obtain sieving.
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| CN201510040786.4A CN104558235B (en) | 2015-01-28 | 2015-01-28 | A kind of manufacture method of high adhered modification guar gum |
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| CN201510040786.4A CN104558235B (en) | 2015-01-28 | 2015-01-28 | A kind of manufacture method of high adhered modification guar gum |
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| CN104558235B CN104558235B (en) | 2017-07-21 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105566508A (en) * | 2016-01-25 | 2016-05-11 | 江苏金和万方新材料科技有限公司 | Preparation method of hydroxyethyl guar gum for cigarette paper |
| CN111440250A (en) * | 2020-05-25 | 2020-07-24 | 刘东辉 | Nonionic tara gum polysaccharide derivative and preparation method and application thereof |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4269975A (en) * | 1980-03-10 | 1981-05-26 | National Starch And Chemical Corporation | Preparation of guar gum |
| CN1367216A (en) * | 2002-03-04 | 2002-09-04 | 无锡金鑫科技有限公司 | Preparation method of high-viscosity nano guar gum |
| WO2012159972A1 (en) * | 2011-05-25 | 2012-11-29 | Lamberti Spa | Hydroxypropyl guar |
| CN103524633A (en) * | 2013-09-28 | 2014-01-22 | 昆山市周市溴化锂溶液厂 | Method for preparing high-viscosity modified guar gum |
| CN103641927A (en) * | 2013-12-10 | 2014-03-19 | 东营金明工贸有限公司 | Method for preparing instant guar gum applicable to continuous blending under low temperature condition |
-
2015
- 2015-01-28 CN CN201510040786.4A patent/CN104558235B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4269975A (en) * | 1980-03-10 | 1981-05-26 | National Starch And Chemical Corporation | Preparation of guar gum |
| CN1367216A (en) * | 2002-03-04 | 2002-09-04 | 无锡金鑫科技有限公司 | Preparation method of high-viscosity nano guar gum |
| WO2012159972A1 (en) * | 2011-05-25 | 2012-11-29 | Lamberti Spa | Hydroxypropyl guar |
| CN103524633A (en) * | 2013-09-28 | 2014-01-22 | 昆山市周市溴化锂溶液厂 | Method for preparing high-viscosity modified guar gum |
| CN103641927A (en) * | 2013-12-10 | 2014-03-19 | 东营金明工贸有限公司 | Method for preparing instant guar gum applicable to continuous blending under low temperature condition |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105566508A (en) * | 2016-01-25 | 2016-05-11 | 江苏金和万方新材料科技有限公司 | Preparation method of hydroxyethyl guar gum for cigarette paper |
| CN111440250A (en) * | 2020-05-25 | 2020-07-24 | 刘东辉 | Nonionic tara gum polysaccharide derivative and preparation method and application thereof |
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| Publication number | Publication date |
|---|---|
| CN104558235B (en) | 2017-07-21 |
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Effective date of registration: 20210210 Address after: 257300 Xiaoli village, Dawang Town, Guangrao County, Dongying City, Shandong Province Patentee after: SHANDONG DEKUN INDUSTRY AND TRADE Co.,Ltd. Address before: 257335 Dongying Jiayi Chemical Co., Ltd., Xiaoli village, Dawang Town, Guangrao County, Dongying City, Shandong Province Patentee before: DONGYING JIAYI CHEMICAL Co.,Ltd. |
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