CN102241068B - Method for semi-continuous dry preparation of organic clay by screw extrusion type kneading machine - Google Patents
Method for semi-continuous dry preparation of organic clay by screw extrusion type kneading machine Download PDFInfo
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Abstract
The invention discloses a method for the semi-continuous dry preparation of organic clay by a screw extrusion type kneading machine, which comprises the following steps: putting smectite clay crude ore powder into a reaction cylinder of the screw extrusion type kneading machine, adding a sodium salt modifying agent, mixing, kneading for 1-10 minutes, adding water in multiple times, and kneading; adding an organic covering agent into the reaction cylinder, raising the material temperature to 60-80 DEG C, keeping the temperature constant, and continuing kneading; and then using acid to regulate the pH value to 3-5, continuing kneading, extruding granular organic clay, and drying. The method has the characteristics of being simple in process flow, being short in consumed time, being low in investment and being high in continuous production efficiency; the method is a clean production method which can save mineral resources, save water, save energy and eliminate sewage emission; and the prepared organic clay is excellent in performance.
Description
Technical field
The present invention relates to a kind of method of semi-continuous dry preparation of organic clay by screw extrusion type kneading machine, specifically, relate to taking Screw Extrusion type kneader as main reactor the method for preparing the organic clay of excellent property under the condition that a small amount of water even do not add water adding, belong to organic clay technical field.
Background technology
Smectite is the Praenomen of 2: 1 inflatable moisture stratiform aluminosilicate clays mineral of type.Comprise dioctahedron and trioctahedron subtribe.In this family, typical mineral comprise wilkinite, saponite, rectorite leng, Hunk holder stone etc.Wherein, taking wilkinite mineral reserves as maximum, processing technology is the most ripe, applies also the most extensive.
Organic clay product is that added value during current smectite family Mineral resources are utilized, technology content are the highest, one series products of tool economic worth, its price is 20-50 times of conventional clay goods, is also a field that needs in-depth development in clay mineral resources development and utilization.
With regard to organic clay production technology, be mainly divided into wet method and two kinds of production methods of dry method according to end-use.As the organobentonite in the fields such as daily-use chemical industry and polymeric modification such as paint, printing ink requires smectite content high, good dispersity, uses wet production, wilkinite is scattered in water, classification, removes impurity, smectite content is increased to 95% or higher, then organic-treating, makes organobentonite.Although the organobentonite quality of this wet processing comparative maturity and preparation is better, but there is following shortcoming in it: the one, and water consumption, use according to statistics on average 15 tons of about water consumptions of one ton of organic clay of wet production, and a large amount of sewage containing acid and tensio-active agent of discharge in process, environment structure is threatened.This is abundant for ore reserve and water resources is relatively deficient northwest, the deep processing of the Northeast's development smectite have produced restriction undoubtedly.The 2nd, resource utilization is low, and being mainly reflected in one ton of organobentonite of general domestic production needs 2.5-3.5 ton wilkinite raw ore, and the wilkinite raw ore that grade is lower consumes more.And the natural sodium bentonite in U.S. Wyoming is produced one ton of organobentonite and only needed 1.5 tons of left and right raw ores, this is mainly to be determined by the objective condition of the bentonite resource type of China.The 3rd, power consumption, the moisture content general requirement < 3% of organic clay product, the link of therefore dewatering in wet method preparation process need to consume a large amount of energy as centrifugal, press filtration, oven dry etc.The 4th, complex process efficiency is low, and wet processing comprises ore dressing, fine ore, pulping, desanding removal of impurities, organically-modified, thickening, dry, abrasive dust etc. step, not only equipment is various, complex process, long reaction time, severe reaction conditions, and invest highly, production efficiency is low.But China's organophilic clay production line is all but to produce with wet processing substantially at present.
For the organic clay in the fields such as oil drilling slurry, environment remediation improvement, casting, focus on use properties, generally do not require high purity, therefore can adopt Semi-dry process (because production process only needs a small amount of moisture, sometimes also referred to as dry production), select applicable smectite ore deposit through dry method ore dressing, removal gangue, pulverizing, original ore powder is directly made organobentonite with organic ammonium intercalation in reactor.The feature of this production technique is exactly that bentonite resource utilization ratio is high, the few and without sewage discharge of water, and with short production cycle, efficiency is high, and energy consumption is low, and cost is low, and competitive power is strong.These are all perfectly in harmony with the low-carbon environment-friendly concept that country is advocating.
The problem existing in order to solve above-mentioned wet processing, Chinese patent CN1446845A discloses a kind of dry-process method for producing bentonite, first it pull an oar wilkinite with doubling bentonitic water, with remove sandstone, and then in mixing roll with soda ash solution by Na-activation of Ca-bentonite With Sodium Compounds, after having retrofited, add again activator activation, finally add organic insulating covering agent, after hybrid reaction completes, then transfer to and on extruser, extrude strip organobentonite.Although it is slightly simplified compared with conventional wet technique, still exist water loss large, complex process, severe reaction conditions, use equipment is loaded down with trivial details, and continuous production is poor, the disadvantage that technique adaptive surface is narrow.
Summary of the invention
The present invention is high in order to solve in prior art wet method organic clay production cost, technical process complexity, resource, the serious problem difficult problem of energy consumption, provide a kind of method of semi-continuous dry preparation of organic clay by screw extrusion type kneading machine, to fill up the blank of prior art.
The method of a kind of semi-continuous dry preparation of organic clay by screw extrusion type kneading machine provided by the invention, comprising:
(1) smectite clay original ore powder is put in Screw Extrusion type kneader reaction cylinder, added the agent of sodium salt remodeling, mixer kneader 1～10min, point several times add water, mediate 5～10min;
(2) in above-mentioned reaction cylinder, add organic insulating covering agent, material temperature is risen to 60～80 DEG C, cover tightly reaction cylinder cap, keep homo(io)thermism, continue to mediate 30～90min; With behind acid for adjusting pH to 3～5, continue to mediate 10～30min afterwards, extrude particulate state organic clay, be drying to obtain;
The mass parts of above-mentioned raw materials is respectively, 100 parts of smectite clay original ore powders, 0～4 part of sodium salt remodeling agent, 20～40 parts, water, 20～60 parts of organic insulating covering agents.
Above-mentioned dried organic clay is through pulverizing, and grading machine desanding, can pack.
Smectite clay in described step (1) can be both dioctahedral montmorillonite (being wilkinite), rectorite leng class clay mineral, also inflatable moisture 2: the 1 type layer aluminosilicate clay minerals such as saponite, Hunk holder stone of three octahedrals.Its purity is sodium base, calcium base, magnesium base or the mixed type high-quality smectite clay mineral that is not less than 60% original ore powder or purifies through screening, desanding, removal of impurities.Preferably raw ore of calcium base bentonite powder, calcium base rectorite leng original ore powder, the natural sodium bentonite of calcium basis soap stone original ore powder or Wyoming.
Be integrated kneading, stirring, the heating of Screw Extrusion type kneader in described step (1), be incubated, vacuumize, mechanical means that the several functions such as screw auger extruding pelletization is integrated, the length-to-diameter ratio of screw rod be not less than 12 and auger outlet add the template that opening diameter is Φ 4mm～Φ 10mm.
The agent of sodium salt in described step (1) remodeling is one or more the mixture in sodium carbonate, Sodium Fluoride, sodium phosphate.
Organic insulating covering agent in described step (2) is the alkyl quaternary ammonium salts Huo quaternary alkylphosphonium salt that single or two long carbochains and carbonatoms are 12～18, and its structure expression is respectively:
R in formula
1carbonatoms is the alkyl of 12-18; R
2for carbonatoms be 1-18 alkyl or benzyl or iso-octyl; R
3for carbonatoms be 1-4 alkyl or hydroxyethyl; R
4for carbonatoms be 1-4 alkyl or hydroxyethyl or thiazolinyl or carboxyl; X is Cl or Br atom.
R in formula
1for the carbonatoms chain alkyl that is 12-18; R
2, R
3, R
4for the carbonatoms alkyl or phenyl that is 1-4; X is Cl or Br atom.
Preferred organic insulating covering agent is one or more the mixture in 16/octadecyl leptodactyline, 16/octadecyl dimethyl benzyl ammonium salt, 16/octadecyl dimethyl iso-octyl ammonium salt, 16/octadecyl dimethyl propylene thiazolinyl ammonium salt, 16/octadecyl dimethyl hydroxyethyl ammonium salt, two dodecyl dimethyl ammonium salt, two octadecyl dimethyl ammonium.
Preferred organic insulating covering agent is that carbonatoms is the mixture of the one or both in chain alkyl tributyl quaternary alkylphosphonium salt or the triphenyl quaternary alkylphosphonium salt of 12-18.
Organic insulating covering agent in described step (2) need be heated and be melted into after liquid in advance, then adds.
Acid in described step (3) is one or more the mixing solutions in sulfuric acid, phosphoric acid, acetic acid, oxalic acid.
The organic clay product of preparation can be applicable to petroleum drilling, casting alcohol-based coating, environmental improvement and reparation, paint and other applicable field.
The Screw Extrusion type kneader that the present invention selects be a kind of integrated kneader and single screw extrusion machine in the mechanical means of one, it both can mediate stirring, shear extrusion, again can heating and thermal insulation, vacuum outgas.Reaction principle of the present invention is under the mixture of organic insulating covering agent and smectite clay mineral is mediated stirring rake at a pair of in the time being warming up to certain temperature in the reaction cylinder of Screw Extrusion type kneader brute force is mediated and stirred, only have under a small amount of moisture participation, it is organic clay that organic cation intercalation enters clay mineral interlayer generation chemical reaction formation organism clay complex, after having reacted, directly pass through the discharging of screw auger extruder grain in reaction cylinder, mechanical shearing and extruding by screw rod in the process of discharging make organic cation react more even with clay mineral lamella, more complete.
The present invention produces one ton of organic clay and only consumes smectite raw ore 0.8-1.2 ton, is significantly less than the consumption of conventional wet, has improved the utilization ratio of Mineral resources.Because preparation process only adds a small amount of water, therefore the water-content of organic clay primary products is generally 10～40%, and product is in the time dehydrating, just not at a large amount of heat energy of needs consumption like this.Whole preparation process one key operation carries out continuously, realizes semi-automation, and production efficiency is high, good product quality.The production that at present this equipment is generally applied to the high-viscosity material such as resin, rubber, polysaccharide with mix.Yet there are no the preparation field that is applied to organic clay.
Beneficial effect
(1) simple, consuming time short, the less investment of preparation method's flow process of the present invention, the high feature of production efficiency continuously; Save the clean preparation method of Mineral resources, water saving, energy-conservation, without sewage discharge;
(2) more even, more complete that reaction carries out that make to organise in the time of auger discharging under the secondary shearing extruding of screw rod, prepares the organic clay product of excellent property.
Brief description of the drawings
Fig. 1 is the X ray diffracting spectrum (XRD) of the raw ore of calcium base bentonite selected in the embodiment of the present invention 1;
Fig. 2 is the X ray diffracting spectrum of the organic clay prepared of the embodiment of the present invention 1.
Specific implementation method
Below in conjunction with embodiment, the present invention is described in further detail and completely, but do not limit content of the present invention.
Raw material part of mentioning in following examples is mass parts.
A method for semi-continuous dry preparation of organic clay by screw extrusion type kneading machine, comprising:
(1) 100 parts of selected raw ore of calcium base bentonite powder are poured in the reaction cylinder of Screw Extrusion type kneader with feeding machine, added 4 parts of sodium carbonate, start kneader, stir 5min, then slowly add 10 parts of water while stirring, stir 10min;
(2) start well heater, add and dissolve into 45 parts of liquid stearyl dimethyl benzyl ammonium chlorides in advance, continue to be stirred to material temperature and rise to 60 DEG C, add water 25 parts, cover tightly cylinder cap, keep 60 DEG C of constant temperature; Continue to stir 60min;
(3) phosphoric acid solution that is 50% by concentration regulates the pH=4 of material, continues 60 DEG C of kneadings of constant temperature, reaction 30min;
(4) start screw auger, extruding particle diameter is the organobentonite particle of 8mm;
(5) by above-mentioned organobentonite particle drying, pulverize, after grading machine classification, pack.
Embodiment 2
Change the calcium-base bentonite in step 1 in embodiment 1 into 100 parts of selected calcium base rectorite leng original ore powders.Other step and embodiment 1 are same.
Embodiment 3
Change the calcium-base bentonite in step 1 in embodiment 1 into 100 parts of selected calcium basis soap stone original ore powders.Other step and embodiment 1 are same.
Embodiment 4
Change the calcium-base bentonite of the step 1 in embodiment 1 into 100 parts of natural sodium bentonites in Wyoming, do not add the agent of any sodium salt remodeling, the organic insulating covering agent in step 2 changes distearyl dimethyl ammonium chloride into, and consumption is 30 parts.Other step and embodiment 1 are same.
Embodiment 5
By the step 2 in embodiment 1, add and dissolve into 55 parts of liquid octadecyl triphenyl phosphonium chlorides in advance, cover tightly cylinder cap, keep 60 DEG C of constant temperature, continue to stir 90min.Other step and embodiment 1 are same
Embodiment 6
Change the particle diameter of extruding of the middle organobentonite particle of step 4 in embodiment 1 into 4mm.Other step is same with enforcement 1.
Embodiment 7
A method for semi-continuous dry preparation of organic clay by screw extrusion type kneading machine, comprising:
(1) 100 parts of selected raw ore of calcium base bentonite powder are poured in a mixing bowl of kneading extruder with batch charger, added 3 parts of Sodium Fluorides, start kneader, stir 5min, then slowly add 10 parts of water while stirring, stir 10min;
(2) start well heater, continue to be stirred to material temperature and rise to 70 DEG C, add and dissolve into 45 parts of liquid octadecyl trimethyl ammonium chloride in advance; Cover tightly stirring cylinder cap, keep 70 DEG C of constant temperature, add 30 parts of water, continue to stir 90min;
(3) phosphoric acid solution that is 50% by concentration regulates the pH=3 of material, continues 70 DEG C of stirrings of constant temperature, reaction 30min;
(4) start screw auger, extruding particle diameter is the organobentonite particle of 6mm;
(5), by organobentonite particle drying, pulverize, pack.
The organic clay of preparation in above-described embodiment 1～7 is carried out to the performance test results and list in table 1.And the organobentonite of preparing with the conventional wet of identical insulating covering agent consumption contrasts.Wherein recording with brookfieldDVII type rheology viscosity apparatus of organic clay stream of gel degree of becoming sticky, solvent is dimethylbenzene, testing rotor is 3#.Other index is all by country or industry standard test.
The contrast of table 1 organic clay properties of sample
Claims (6)
1. a method for semi-continuous dry preparation of organic clay by screw extrusion type kneading machine, comprising:
(1) smectite clay original ore powder is put in Screw Extrusion type kneader reaction cylinder, added the agent of sodium salt remodeling, mixer kneader 1～10min, gradation adds water, mediates 5～10min; Wherein, Screw Extrusion type kneader has been integrated kneading, stirring, heating, be incubated, vacuumize, mechanical means that screw auger extruding pelletization is integrated, the length-to-diameter ratio of screw rod be not less than 12 and auger outlet add the template that opening diameter is Φ 4mm～Φ 10mm; Smectite clay is saponite or the Hunk holder stone of dioctahedral montmorillonite, rectorite leng class clay mineral, three octahedrals; Its purity is sodium base, calcium base, magnesium base or the mixed type smectite clay mineral that is not less than 60% original ore powder or purifies through screening, desanding, removal of impurities;
(2) in above-mentioned reaction cylinder, add organic insulating covering agent, material temperature is risen to 60～80 DEG C, cover tightly reaction cylinder cap, keep homo(io)thermism, continue to mediate 30～90min; With behind acid for adjusting pH to 3～5, continue to mediate 10～30min afterwards, extrude particulate state organic clay, be drying to obtain; Wherein, organic insulating covering agent is one or more the mixture in 16/octadecyl leptodactyline, 16/octadecyl dimethyl benzyl ammonium salt, 16/octadecyl dimethyl iso-octyl ammonium salt, 16/octadecyl dimethyl propylene thiazolinyl ammonium salt, 16/octadecyl dimethyl hydroxyethyl ammonium salt, two dodecyl dimethyl ammonium salt, two octadecyl dimethyl ammonium; The mass parts of above-mentioned raw materials is respectively, 100 parts of smectite clay original ore powders, 0～4 part of sodium salt remodeling agent, 20～30 parts, water, 20～60 parts of organic insulating covering agents.
2. the method for a kind of semi-continuous dry preparation of organic clay by screw extrusion type kneading machine according to claim 1, is characterized in that: described smectite clay original ore powder is raw ore of calcium base bentonite powder, calcium base rectorite leng original ore powder, the natural sodium bentonite of calcium basis soap stone original ore powder or Wyoming.
3. the method for a kind of semi-continuous dry preparation of organic clay by screw extrusion type kneading machine according to claim 1, is characterized in that: the agent of sodium salt in described step (1) remodeling is one or more the mixture in sodium carbonate, Sodium Fluoride, sodium phosphate.
4. the method for a kind of semi-continuous dry preparation of organic clay by screw extrusion type kneading machine according to claim 1, is characterized in that: the organic insulating covering agent in described step (2) need be heated in advance and is melted into liquid.
5. the method for a kind of semi-continuous dry preparation of organic clay by screw extrusion type kneading machine according to claim 1, is characterized in that: the acid in described step (2) is one or more the mixing solutions in sulfuric acid, phosphoric acid, acetic acid, oxalic acid.
6. the method for a kind of semi-continuous dry preparation of organic clay by screw extrusion type kneading machine according to claim 1, is characterized in that: the organic clay of described step (2) gained is applied to petroleum drilling, casting alcohol-based coating, environmental improvement and reparation or paint field.
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| CN102653697B (en) * | 2011-12-21 | 2013-08-21 | 东昊石油集团有限公司 | Special industrial lubricant for cement mixer and reduction box, and method for preparing special industrial lubricant |
| CN105936510B (en) * | 2014-10-14 | 2018-08-24 | 北京京盛国泰科技有限公司 | A kind of bentonite method of modifying |
| CN105087912B (en) * | 2015-08-31 | 2017-05-31 | 中南大学 | A kind of iron ore pellets humic acid method for preparing modified bentonite and its application |
| CN105087916B (en) * | 2015-08-31 | 2017-09-26 | 中南大学 | A kind of method that ferric manganese ore concentrate prepares oxide pellet |
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