CN1266230C - Smectite organogel and its preparing method - Google Patents

Smectite organogel and its preparing method Download PDF

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CN1266230C
CN1266230C CN 200410079073 CN200410079073A CN1266230C CN 1266230 C CN1266230 C CN 1266230C CN 200410079073 CN200410079073 CN 200410079073 CN 200410079073 A CN200410079073 A CN 200410079073A CN 1266230 C CN1266230 C CN 1266230C
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smectite
organogel
inorganic gel
slurries
reaction
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CN1621454A (en
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王道容
匡军
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Abstract

The present invention relates to smectite organogel and a preparing method thereof. Smectite minerals, such as magnesium hectorite, are used as raw material. After prepared, smectite inorganic gel is processed particularly by the following steps: 1. the smectite inorganic gel is acidified and activated; 2. organic coverage reaction is implemented under ultrasonication; 3 the smectite organogel obtained by the reaction of the steps is filtered, washed, dried, pulverized, etc. to obtain a final smectite organogel product. The product is better than organic bentonite gel on main performance, can be used as cosmetics, printing ink, a lubricant thickening agent, a paint suspending agent, an oily coating thickening agent, a petroleum well drilling oil-base mud, a releasing stuck agent, etc. and has wide purposes in grease, chemical industry and petroleum industry.

Description

Smectite organogel and preparation method thereof
Technical field
The invention belongs to a kind of organic clay gelatinous material, particularly a kind of is the smectite organogel and preparation method thereof of feedstock production with the smectite clay.
Background material
Wilkinite is to be the genus dioctahedron laminate structure clay mineral of main component with the montmorillonite; Smectite is the clay mineral with trioctahedron laminate structure.Wilkinite is in China and reserves are very abundant in the world, and has the smectite ore deposit reserve of industrial value extremely rare.Wilkinite has good special performances such as good water swelling, colloidal stability, suspension and thickening property; And smectite has the nearly all performance of wilkinite, and all more superior on most of performances.The smectite mineral can include magnesium hectorite, magnesium soap stone, lithium magnesium soap stone (Hunk holder stone), griffithite and aluminium soap stone etc. according to feature metal ion difference, all are the smectites with trioctahedron laminate structure, and are different from the montmorillonite of dioctahedron laminate structure.Because the special construction and the premium properties of smectite, prepared inorganic gel is better than the inorganic gel performance of wilkinite preparation, be used for fields such as medicine, makeup, special coating, agricultural chemicals widely, but can only in aqueous phase system, use, particularly can't use in the organic system, range of application is restricted.
Existing is that the wilkinite of essential mineral composition prepares organobentonite in order to the dioctahedron montmorillonite generally, and its preparation technology is existing open, discloses a kind of method for preparing organobentonite as CN1052094A and has been: (1), preparation hydrogen type bentonite; (2), cover reaction with organic insulating covering agent and hydrogen type bentonite; (3) filtration, washing, drying, pulverizing obtain the organobentonite product.
Chinese patent application number: 2004100398405 have proposed a kind of " preparation method of high purity silicic acid magnalium inorganic gel ", be that a kind of neusilin mineral of magnesium hectorite that comprise prepare the method for inorganic gel, but do not see the public publish for preparing the smectite organogel method with the trioctahedron smectite.
In order to enlarge the application of trioctahedron smectite in organic system, the objective of the invention is to prepare smectite organogel with the smectite inorganic gel; Another object of the present invention provides the preparation method of smectite organogel.
Summary of the invention
In order to achieve the above object, the present invention adopts preparation method's step to be:
1, acid activation smectite inorganic gel: with deionized water preparation solid content is the smectite inorganic gel slurries of 3-6%, add mineral acid (mineral acid be in hydrochloric acid, sulfuric acid, the nitric acid any), the adding mineral acid quantity is 0.5-10 a times of smectite inorganic gel slurry solid content, make PH=1-3, under 20-40 ℃ of temperature, stirring reaction 1-5 hour, obtain acid activation smectite inorganic gel slurries.
2, the organic covering reaction of ultrasonic wave: with acid activation smectite inorganic gel slurries, be mixed with the slurries that concentration is 1-4% with deionized water, add the organic insulating covering agent of quaternary ammonium salt, add-on is the 20-80% of acid activation smectite inorganic gel slurry solid content, under the ultrasonic wave effect, carry out organic covering reaction, temperature of reaction is 40-80 ℃, and the reaction times is 0.5-1.5 hour.Described organic insulating covering agent be dodecyl to the octadecyl quaternary ammonium salt, best is palmityl trimethyl ammonium chloride, octadecyl dimethyl Bian ammonium chloride, two octadecyl Bian Ji alkyl dimethyl ammonium chloride; Described ultrasonic frequency is 20-60KHZ, and power is 350-1500W.Reaction obtains the smectite organogel slurries.
3, aftertreatment: the smectite organogel slurries with above-mentioned two-step reaction obtains through filtration, washing, dry, pulverizing, obtain the finished product.
It is shorter that the present invention prepares the smectite organogel reaction times, and reaction is thorough, and quality product is better, and outward appearance is more transparent, and kinetic viscosity is higher.The concrete testing method of its kinetic viscosity is as follows:
Take by weighing smectite organogel sample 3.6 grams, put into container, add 54 milliliters of dimethylbenzene, start stirring, being 2100 rev/mins at rotating speed stirred 5 minutes down, add 1.5 ml methanol, being 3500 rev/mins at rotating speed stirred 5 minutes down, stop to stir, take out sample, use NDJ-79 type rotational viscosimeter immediately, the kinetic viscosity that records smectite organogel when rotating speed is 750 rev/mins is 4.3-4.8 handkerchief second, records preferably that the bentonite kinetic viscosity is 2.5-4.2 handkerchief second and use the same method.
Description of drawings
Accompanying drawing 1 is a process flow sheet of the present invention
Accompanying drawing 2 is the embodiments of the invention process flow sheet
Embodiment
Below in conjunction with drawings and Examples the present invention is further described specifically.
Embodiment: see shown in the accompanying drawing 2 that a kind of magnesium hectorite organogel follows these steps to be prepared:
1, acid activation magnesium hectorite inorganic gel: be 3% magnesium hectorite inorganic gel slurries with magnesium hectorite inorganic gel and deionized water preparation solid content, the 3-6 hydrochloric acid doubly that adds magnesium hectorite inorganic gel slurry solid content, make PH=1-3,25-30 ℃ was stirred 3 hours down, obtains acid activation magnesium hectorite inorganic gel slurries.
2, the organic covering reaction of ultrasonic wave: with the acid activation magnesium hectorite inorganic gel slurries of above-mentioned steps acquisition, be mixed with solid content and be 2% slurries, the palmityl trimethyl ammonium chloride that adds the 25-35% of slurry solid content, in ultrasonic unit, carry out the organic covering reaction of ultrasonic wave, under 60 ℃ temperature, reacted 1-1.2 hour, and obtained magnesium hectorite organogel slurries.Described ultrasonic frequency is 59KHZ, and power is 350W.
3, the magnesium hectorite organogel slurries that above-mentioned steps is obtained filter, wash (to there not being chlorion), drying, pulverize, are screened to 200 orders, are prepared into magnesium hectorite organogel product.
By the magnesium hectorite organogel that above-mentioned steps makes, the kinetic viscosity that records was 4.5 handkerchief seconds.The measuring method of its kinetic viscosity is:
Take by weighing magnesium hectorite organogel sample 3.6 grams, put into container, add 54 milliliters of dimethylbenzene, start stirring, be 2100 rev/mins at rotating speed and stirred 5 minutes down, add 1.5 ml methanol, be 3500 rev/mins at rotating speed and stirred 5 minutes down, stop to stir, take out sample, use NDJ-79 type rotational viscosimeter immediately, the kinetic viscosity that records magnesium hectorite organogel when rotating speed is 750 rev/mins was 4.5 handkerchief seconds.

Claims (1)

1, a kind of preparation method of smectite organogel, smectite organogel slurries with the preparation of smectite inorganic gel, through filtration, washing, drying, pulverizing, aftertreatment, its feature part is to prepare the smectite organogel slurries with the smectite inorganic gel to comprise the steps:
(1) acid activation smectite inorganic gel: with deionized water preparation solid content is the smectite inorganic gel slurries of 3-6%, add any mineral acid in hydrochloric acid, sulfuric acid, the nitric acid, the adding mineral acid quantity is 0.5-10 a times of smectite inorganic gel slurry solid content, make PH=1-3, under 20-40 ℃ of temperature, stirring reaction 1-5 hour, obtain acid activation smectite inorganic gel slurries;
(2) the organic covering reaction of ultrasonic wave: with acid activation smectite inorganic gel slurries, be mixed with the slurries that concentration is 1-4% with deionized water, add and to be selected from 12 organic insulating covering agents of any quaternary ammonium salt to the octadecyl quaternary ammonium salt, add-on is the 20-80% of acid activation smectite inorganic gel slurry solid content, in frequency is that 20-60KHZ, power are to carry out organic covering reaction under the ultrasonic wave effect of 350-1500W, reaction is 0.5-1.5 hour under 40-80 ℃ of temperature, obtains the smectite organogel slurries.
CN 200410079073 2004-09-29 2004-09-29 Smectite organogel and its preparing method Expired - Fee Related CN1266230C (en)

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CN1266230C true CN1266230C (en) 2006-07-26

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Families Citing this family (9)

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Publication number Priority date Publication date Assignee Title
CN102584055B (en) * 2012-02-29 2013-08-07 浙江丰虹新材料股份有限公司 Smectite inorganic gel particles easy to disintegrate and disperse in water and preparation method of smectite inorganic gel particles
CN104059625B (en) * 2014-07-02 2017-02-15 成都理工大学 Method for preparing high-stability heat-resistance and salt-tolerance air foam oil displacing agent
CN105753004B (en) * 2016-01-26 2017-12-26 武汉华矿胶体化学有限公司 A kind of organic clay and its production method of big interplanar distance
CN105800753B (en) * 2016-04-05 2018-06-19 江苏海明斯新材料科技有限公司 A kind of preparation method of environmentally protective high-performance lithium saponite lacquer mist coagulant
CN105954148A (en) * 2016-04-26 2016-09-21 重庆鹏凯精细化工有限公司 Method for determination of viscosity generation and dissolution time of dissolution-retarding non-ionic cellulose ether
US9637614B1 (en) * 2016-06-22 2017-05-02 Byk Usa Inc. Process of manufacturing thickeners and the use of thus produced thickeners in high-viscosity unsaturated polyester containing formulations
CN106745013A (en) * 2016-12-27 2017-05-31 江南大学 A kind of lithium magnesium silicate compound and preparation method thereof
CN108342252B (en) * 2018-01-19 2021-05-28 中山职业技术学院 Method for efficiently extracting agilawood essential oil
CN110343267A (en) * 2019-07-24 2019-10-18 安吉艾格赛思生物科技有限公司 A kind of hectorite inorganic gel and application thereof

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