CN105753004B - A kind of organic clay and its production method of big interplanar distance - Google Patents
A kind of organic clay and its production method of big interplanar distance Download PDFInfo
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- CN105753004B CN105753004B CN201610053343.3A CN201610053343A CN105753004B CN 105753004 B CN105753004 B CN 105753004B CN 201610053343 A CN201610053343 A CN 201610053343A CN 105753004 B CN105753004 B CN 105753004B
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/20—Silicates
- C01B33/36—Silicates having base-exchange properties but not having molecular sieve properties
- C01B33/38—Layered base-exchange silicates, e.g. clays, micas or alkali metal silicates of kenyaite or magadiite type
- C01B33/44—Products obtained from layered base-exchange silicates by ion-exchange with organic compounds such as ammonium, phosphonium or sulfonium compounds or by intercalation of organic compounds, e.g. organoclay material
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
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Abstract
A kind of organic clay and its production method of big interplanar distance, are made up of rectorite and double long-chain alkyl quaternary ammonium salt, and its weight is：Rectorite 46~81, double long-chain alkyl quaternary ammonium salt 19~54.Its production craft step is：A, inorganic acid activating pretreatment；B, double long-chain alkyl quaternary ammonium salt organises reaction；C, filtering, ageing, drying, crushing.It is characteristic of the invention that, using rectorite as raw clay, using the quaternary ammonium salt containing double long-chain alkyl as organic modifiers, organised using inorganic acid activating pretreatment, high temperature wet, filter the processes such as ageing drying and crushing as production technology, the interplanar distance d [001] of obtained organic clay product can reach 4.5~5nm, and interplanar distance significantly increases.In drilling fluid field, the Organoclay Products of the big interplanar distance of the present invention can be used as white oil, refined mineral oil, the colloidal materials for synthesizing the low toxic and environment-friendly type drilling fluid such as base oil product, have the characteristics that into that colloidality is good, rheological characteristic is good, filter loss low and high temperature excellent in stability.
Description
Technical field
The present invention relates to a kind of composition of organic clay and production technology, more particularly to a kind of organic rectorite and its production
Method.Meanwhile the present invention also relates to the industries such as a kind of oil, natural gas, Di Kuang, architectural engineering to be used for drilling fluid, completion fluid
Colloidal materials.
Background technology
First, the realization means of the organic clay of big interplanar distance
Organic clay industrially can be widely applied to petroleum drilling fluid, coating, polymer nanocomposites and other
Field of fine chemical.By the clay of organic modification, its original interplanar distance becomes big.In fields such as drilling fluid, rheological agents,
The interplanar distance positive correlation of the suspension of colloidal dispersion, rheological characteristic and organic clay.It is organic viscous in polymer composites field
The interplanar distance of soil is bigger, and clay-phase is more easily peeled off slabbing and is dispersed among polymeric matrix, so as to improve material property.
The component of organic clay is typically made up of raw clay, organic modifiers, is also needed to add some sometimes in component and is helped
Agent, to promote the reaction that organises, or improve application performance.
The raw material of existing organic clay is based on swelling great soil group.Bentonitic main component is montmorillonite.According to montmorillonite layer
Between cation different type, its interplanar distance d [001] is generally 1.2~1.5nm；If without interlayer cation, d [001] is then
0.96nm.Bentonite d [001] can reach more than 2nm.
The approach of increase interplanar distance has two.One approach is the appropriate organic modifiers for selecting molecular weight bigger, such as
Double long-chain alkyl quaternary ammonium salt can provide bigger molecular weight, regrettably, in the world in known clay mineral reserve, only a small number of ore deposits
Tibetan is suitable for using double long-chain alkyl quaternary ammonium salt organically-modified, and the unsuitable double long-chain alkyl quaternary ammonium salt of most of bentonite is organic to be changed
Property；Another approach is the bigger clay of the initial interplanar distance of selection, and the d [001] of rectorite is 2.2~2.7nm, is known
One of maximum clay mineral of original interplanar distance in various clays, it is to improve interplanar distance to prepare organic clay as raw material using it
Effective way.
Patent 02115758.8 discloses a kind of organic composite rectorite and preparation method thereof, organic rectorite therein by
Rectorite, organic intercalation agent (such as amino acid of long chain alkyl ammonium salt, hexamethylene diamine adipate or carbon number 6~12), proton
Agent forms.So-called organic intercalation agent is organic modifiers.For example, alleged long chain alkyl ammonium salt intercalator is hexadecane
Base amine, cetyl trimethyl amine (sic) or carbon number are 12~18 other long chain alkyl ammonium salts, for single length
Alkyl quaternary ammonium salts, the organic intercalation agent that every 100 parts of rectorites add at most can be to 30 parts.Even if using purity more than 90%
Rectorite is raw material, and obtained organic rectorite interplanar distance d [001] highest is only capable of reaching 3.8~4.1nm.
Patent 02115876.2 discloses a kind of rectorite organic compound and its system for synthesizing nano compound material
Preparation Method, its organic rectorite compound are organic by rectorite and amine or amine salt, amino acid, lactams, diamine diacid salt etc.
Monomer or organic monomer and protonating agent occur ion-exchange reactions and are made.According to document, " rectorite is compound in polymer nanocomposite
Application in material " (《Engineering plastics application》2004, volume 32, the 1st phase) report, using the technology, through organic cation
The interplanar distance d [001] of High-purity Rectorite/organic double compound obtained by exchange reaction is brought up to by 2.2616nm
4.2924nm。
Organic rectorite is by clay/three kinds of organic modifiers/protonating agent component or clay/organic in above-mentioned two patent
Two kinds of components of modifying agent are formed, and organic modifiers therein do not include the quaternary ammonium salt of double long-chain alkyl, and modifier molecules amount is still not
Sufficiently high, its product that organises is not easy to obtain bigger interplanar distance.
It is public as the example that organic rectorite is prepared using ultrahigh molecular weight as organic modifiers, patent 200610124484.6
A kind of nano composite material of quaternary ammonium salt of chitosan/rectorite and preparation method thereof is opened, the composite is substantially that one kind has
Machine rectorite, basic composition is chitosan quaternary ammonium salt and rectorite, and using chitosan quaternary ammonium salt as organic modifiers, support is tired out after intercalation
Stone interplanar distance d [001] is between 2.9nm~3.5nm.Another includes about chitosan quaternary ammonium salt organic modifiers
The patent of machine rectorite is 200910213896.0, and organic modifiers used are carboxymethyl chitosan quaternary ammonium salt, its organic tired support
The interplanar distance d [001] of stone is between 4.2nm~4.72nm.But chitosan class quaternary ammonium salt is with high costs, its is organic tired
Stone product orientation is ask not possess and applied in fields such as oil drilling, coating, engineering plastics, rubber in medical material, biomaterial
Economy.
Patent 201010258856.0, patent 201510893277.6, patent 201511005536.3 disclose it is several not
Same oil base drilling fluid organic rectorite and its production method, organic rectorite therein are all by rectorite and single long alkane
Based quaternary ammonium salt is formed, and it is m- alkyl trimethyl halogen that its claim, the content of the invention, which illustrate general term used quaternary ammonium salt-modified dose,
Change ammonium or n- alkyl-dimethyl benzyl ammonium halides.Therefore, with regard to organic modifiers molecular weight contrastingly, it organises product not
Easily obtain bigger interplanar distance.
If using this brand-new component of rectorite/double long-chain alkyl quaternary ammonium salt, produced eventually with regard to its organic clay can be improved
The interplanar distance of product, previously described two approach for improving organic clay interplanar distance are all achieved, and this is exactly the present invention
Products innovation place.Rectorite is a kind of new interbed silicate mineral, in its crystal structure, class montmorillonite layer
With class mica layer with 1:1 rule is staggered.The d [001] of natural accumulation supporting stone is the two of 2.2~2.7nm, about montmorillonite
Times.Rectorite layer charge is moderate, both with good ion exchangeable, can have good scattered fissility.Using appropriate
Technique, rectorite are suitable for carrying out organic modification with the organic modifiers of the macromolecules such as double long-chain alkyl quaternary ammonium salt.
2nd, meaning of the big interplanar distance organic clay to low toxic and environment-friendly non-aqueous drilling fluids
In oil drilling process, non-water-base drilling fluid (NADFs)-i.e. oil base and synthetic base drilling fluid-in petroleum industry
Application it is more and more extensive, before the base fluid of oil base drilling fluid system based on diesel oil base.However, diesel oil aromatic hydrocarbon content compared with
Height, it is unfavorable for environmental protection.In recent years, to reduce drilling cuttings discharge to the influence caused by environment, there is degradable, low stain environmental protection
The less toxic mineral oil (white oil) of type, high refined mineral oil and synthesize base (ester, alkane, alkene) drilling fluid application it is more and more wider
It is general.Oil base drilling fluid and synthetic base drilling fluid beyond diesel oil, low toxic and environment-friendly type drilling fluid can be referred to as.However, these are less toxic
The system feature of Environment-protecting Drilling Fluids is that viscosity is low, aromatic content is low, and organic clay for oil base drilling fluid in the market is made
For the gelation, filtration reduction, thickening of the oleophylic colloid of low toxic and environment-friendly system, to put forward cutting property generally poor.
According to the colloid chemistry principle of drilling fluid, the bigger interplanar distance of organic clay crystal structure is advantageous to them low
Good colloidal property, rheological characteristic, suspending stabilized performance are played in poison ring protection drilling fluid system.
Therefore, in this important applied field of drilling fluid, big interplanar distance organic clay is to low toxic and environment-friendly non-aqueous drilling fluids
It is significant.
The content of the invention
Structures shape performance.For the shortcoming on the crystal structure of existing organic clay, the invention discloses one kind to have
The new organic clay and its production method of big interplanar distance, to meet the industrially requirement to high-performance organic clay,
The especially requirement of low toxic and environment-friendly type oil base and synthetic base drilling fluid system to organic clay.
Therefore, the present invention uses organic modifiers of the double long-chain alkyl quaternary ammonium salt for rectorite.In order to quantify to match somebody with somebody exactly
Side, we use the quaternary ammonium salt loading addition Q of the organic rectorite of the disclosed mistake of inventor of this patent calculation formula：
Q=0.073776 × M × p × (1-wr) ÷ (1-wq)
In formula,
During Q-organise reaction, the saturation addition (kg) of quaternary ammonium salt is used per 100kg rectorites；
The molecular weight of M-used quaternary ammonium salt；
P-rectorite purity, number range 0~1；
Wr-rectorite water content, number range 0~1；
Wq-quaternary ammonium salt water content, number range 0~1.
According to the present invention product component in rectorite, double long-chain alkyl quaternary ammonium salt industrial raw material usual conditions,
The situation of maximum quaternary ammonium salt addition：P=98.0%, wr=6.5%, wq=50%, non-alkyl active group are benzyl, quaternary ammonium salt species
For double tetracosyl methyl-benzyl ammonium bromides (molecular weight 874), Q=118.2, i.e. 100 parts of rectorites add quaternary ammonium salt 118.2
Part, that is, 45.9 parts of rectorites add 54.1 parts of quaternary ammonium salts, after rounding, obtain rectorite:Quaternary ammonium salt=46:54.Minimum of the invention
The situation of quaternary ammonium salt addition：P=65.0%, wr=6.5%, wq=90%, quaternary ammonium salt species are double dodecyldimethylamine ammonium chlorides
(molecular weight 473), Q=23.6, i.e. 100 parts of rectorites add 23.6 parts of quaternary ammonium salt, that is, 80.9 parts of rectorites add 19.1 parts of seasons
Ammonium salt, after rounding, obtain rectorite:Quaternary ammonium salt=81:19.
So the organic clay of the big interplanar distance of patent of the present invention is made up of rectorite and double long-chain alkyl quaternary ammonium salt,
Its weight is：Rectorite 46~81, double long-chain alkyl quaternary ammonium salt 19~54, added equivalent to every 100 parts of rectorites double
23.6~118.2 parts of long chain alkyl ammonium salt.
Production craft step of the present invention is：
(1) inorganic acid activating pretreatment：Inorganic acid aqueous solution 400 is added in the container for filling the parts by weight of rectorite 100
~600 parts by weight, the inorganic acid aqueous solution are the sulfuric acid of 1~2% concentration or the hydrochloric acid of 0.4~1.0% concentration, then heat to 60
~80 DEG C, 30~210min, speed of agitator 120rpm are stirred, forms uniform slurries, is placed 8~48 hours, then filter-press dehydration,
Obtain inorganic acid Activated Rectorite；
(2) it is organically-modified：Inorganic acid Activated Rectorite is put into container, added equivalent to 1~20 times of rectorite weight
Water stirring be slurries, take concentration to be added to slurries for 50~90% parts by weight of double long-chain alkyl quaternary ammonium salt 23.6~118.2
In, continuing to stir and heat, reaction temperature is set in 70~115 DEG C, 30~210min of insulated and stirred, speed of agitator 120rpm,
Obtain mixed serum.
（3）Finished product：100-400 parts by weight water is added in mixed serum, after stirring 1~3min, filtering, ageing, done
Dry, crushing, obtain the finished product of big interplanar distance organic clay.
Rectorite raw material is calcium type, and purity is 65~98%, and the calcium ion accounting in interlayer cation reaches more than 50%.
Double long-chain alkyl quaternary ammonium salt is double m alkyl-dimethyl-ammonium halide or double n Alkyl-methyls-non-alkyl active group-halogen
Change ammonium, m, n are the carbon number of double carbochains, and its value is 14~24, and halogen is chlorine or bromine, and non-alkyl active group is alcoxyl
One kind in base, carbonyl, carboxyl, benzyl.
Filtering is after adding water to stir the product mixed serum for the reaction that organises, to move into common plate and frame filter press, barrier film
Filter press, vacuum filtration machine or centrifuge, filter off moisture and soluble ion.
Ageing is that the filter cake after filtering or similar dehydration product are placed at shady and cool ventilation to stack 8~48 hours.
Drying is that the product after ageing is dried into moisture content≤3.5% under 100~150 DEG C of environment.
Crushing is that dried product is ground into at least 80 mesh or average grain diameter≤0.173mm using pulverizer.
In summary, process route of the invention be inorganic acid activation-high temperature wet method organise-carry be aged process after
Processing, it is the process route for the innovation for preparing organic rectorite.
After inorganic acid activation, the increase of rectorite specific surface area, a part of Al, Mg ion can be also dissolved, is added
The exchangeable cationic type between layer amount.Inorganic acid activating pretreatment technique is also adsorbed organic in addition to increase cation exchange space
The effect of cation.The preconditioning technique is beneficial to the cation exchange reaction of macromolecule organic modifiers, beneficial in dispersion
Thicker, more stable micelle is formed in system.The present invention uses double long-chain alkyl quaternary ammonium salt therefore, to there is pin as organic modifiers
The preconditioning technique of inorganic acid activation is employed to property.
Using the formula and production technology of the present invention, previously described two approach for improving organic clay interplanar distance are all
It is achieved.The d [001] for the Organoclay Products that XRD is measured is 4.5~5nm, all organic tired higher than disclosed in the past
Stone class organic clay is held in the palm, wherein also including the organic rectorite of chitosan quaternary ammonium salt.
Organic clay prepared by the present invention, in low toxic and environment-friendly type drilling fluid system, with good into colloidality, rheology
Property, filtration reduction, high-temperature stability.
Because rectorite cation exchange capacity (CEC) is about the half of montmorillonite, therefore organic modifiers dosage is relatively fewer.By this
The formula of invention uses the bigger double long-chain alkyl quaternary ammonium salt of molecular weight, and for organic modifiers, its totle drilling cost is not high.
Brief description of the drawings
Fig. 1 is the small angle x-ray diffraction (SAXD) figure of embodiment sample, and 2 θ angular ranges are 0.5 °~10 °.
Embodiment
Embodiment 1. weighs 100 parts of the calcium base rectorite fine ore of purity 70%, is added to the sulfuric acid that 400 parts of concentration are 1.5%
In solution, stirring, 80 DEG C are then heated to, continue to stir 60min, form uniform slurries, place 36 hours, then press filtration takes off
Water.Filter cake is taken out, is put into container, is added with 500 parts of water, heats and is stirred with 120rpm speed, temperature is risen to 75 DEG C.Take net
36.5 parts of the double hexadecyl trimethyl ammonium chloride of content 70%, add container, vessel temp is maintained at 75 DEG C, continue with
120rpm speed stirring, organise reaction 90min.200 parts of water are added, stir 2min.Slurries are imported into filter press, press filtration,
Sample is taken out, is placed 24 hours, being dried to water content under the conditions of 120 DEG C is down to 3%.200 mesh (0.074mm) are crushed to, are made
The organic clay of the big interplanar distance of embodiment 1.Low-angle XRD results are shown in Fig. 1, d [001]=4.5155nm；Measure white oil system
Mud property parameter is shown in Table 1.
Embodiment 2. weighs 100 parts of the calcium base rectorite fine ore of purity 75%, and it is molten to be added to the hydrochloric acid that 500 parts of concentration are 1%
In liquid, stirring, 80 DEG C are then heated to, continue to stir 60min, form uniform slurries, place 48 hours, then filter-press dehydration.
Filter cake is taken out, is put into container, is added with 600 parts of water, heats and is stirred with 120rpm speed, temperature is risen to 85 DEG C.Add net
40.3 parts of double octadecyl methyl benzyl ammonium chlorides of content 85%, are incubated and continue to stir, and organise reaction 90min.Add
200 parts of water, stir 2min.Slurries are imported into filter press, press filtration, sample is taken out, places 24 hours, dried under the conditions of 120 DEG C
3% is down to water content.200 mesh (0.074mm) are crushed to, the organic clay of the big interplanar distance of embodiment 2 is made.Low-angle
XRD results are shown in Fig. 1, d [001]=4.8106nm；Measure white oil system mud performance parameter and be shown in Table 1.
Embodiment 3. weighs 100 parts of the calcium base rectorite powder of purity 92%, is added to the sulfuric acid solution that 400 parts of concentration are 1.5%
In, stirring, 80 DEG C are then heated to, continue to stir 60min, form uniform slurries, place 48 hours, then filter-press dehydration.Take
Go out filter cake, be put into container, be added with 800 parts of water, heat and stirred with 120rpm speed, temperature is risen to 110 DEG C.Addition contains only
57.2 parts of the DDA of amount 75%, insulation, and pressure is established in closed container, continue with 120rpm
Speed stirring, organise reaction 90min.200 parts of water are added, stir 2min.Slurries are imported into filter press, press filtration, take out sample
Product, are placed 24 hours, and being dried to water content under the conditions of 120 DEG C is down to 3%.200 mesh (0.074mm) are crushed to, embodiment is made
The organic clay of 3 big interplanar distance.Low-angle XRD results are shown in Fig. 1, d [001]=5.0151nm；Measure white oil system mud
Energy parameter is shown in Table 1.
The performance test results (5# white oils) of the embodiment of table 1
Note：
1. colloidity determines：At 25 DEG C of room temperature, weigh 4.0g samples and be put into 200ml No. 5 white oils with 4000rmp speed
2min is stirred with fully dispersed, therefrom takes 100ml to be placed in tool plug graduated cylinder, upper and lower hand 5min is remaining to press SY/T 6615-2005
Attached B is performed, and record sample stands 90min numerical value.
2. rheology measurement：10.5g organic rectorites are taken, are poured into the mud cap for No. 5 white oils for filling 350ml,
10min is stirred under 4000rpm, removes mud cap, scrapes off and is adhered to container side wall, the sample of bottom surface.Again in 11000rpm rotating speeds
Lower stirring 10min.It is remaining to be performed by the attached B of SY/T 6615-2005.
3. filter loss determines：380ml No. 5 white oils, add 20ml distilled water, add 12.0g organic rectorites, in 4000rpm
Lower stirring 10min, removes mud cap, scrapes off and is adhered to container side wall, the rectorite of bottom surface.Then, under 11000rpm rotating speeds
Stir 10min.It is remaining to be performed by the attached B of SY/T 6615-2005.
4. high temperature rheology, high temperature filter loss determine：Sample, stirring as stated above, complete 11000rpm therein and turn
After the lower stirring of speed, sample loads stainless cylinder of steel, is filled with 1.0MPa nitrogen, 180 DEG C of heat rolling 16h, takes out, be cooled to 25 DEG C of room temperatures,
5min is stirred under 11000rpm rotating speeds, by the attached B flow measurements denaturation of SY/T 6615-2005 and filter loss.
Claims (7)
1. a kind of production method of the organic clay of big interplanar distance, it is characterised in that it is by rectorite and double long-chain alkyl quaternary ammonium
Salt forms, and its weight is：Rectorite 46~81, double long-chain alkyl quaternary ammonium salt 19~54；Its production craft step is：
(1) inorganic acid activating pretreatment：In the container for filling the parts by weight of rectorite 100 add inorganic acid aqueous solution 400~
600 parts by weight, the inorganic acid aqueous solution are the sulfuric acid of 1~2% concentration or the hydrochloric acid of 0.4~1.0% concentration, then heat to 60~
80 DEG C, 30~210min, speed of agitator 120rpm are stirred, forms uniform slurries, is placed 8~48 hours, then filter-press dehydration, obtain
Inorganic acid Activated Rectorite；
(2) it is organically-modified：Inorganic acid Activated Rectorite is put into container, adds water of 1~20 times equivalent to rectorite weight
Stirring as slurries, the parts by weight of double long-chain alkyl quaternary ammonium salt 23.6~118.2 for taking concentration to be 50~90% are added in slurries, after
Continuous to stir and heat, reaction temperature is set in 70~115 DEG C, 30~210min of insulated and stirred, speed of agitator 120rpm, must mix
Slurries；
（3）Finished product：100~400 parts by weight water are added in mixed serum, after stirring 1~3min, filter, be aged, drying,
Crush, obtain big interplanar distance organic clay finished product.
A kind of 2. production method of the organic clay of big interplanar distance according to claim 1, it is characterised in that rectorite
For calcium type, purity is 65~98%, and the calcium ion accounting in interlayer cation reaches more than 50%.
A kind of 3. production method of the organic clay of big interplanar distance according to claim 2, it is characterised in that double long-chains
Alkyl quaternary ammonium salts is double m alkyl-dimethyl-ammonium halide or double n Alkyl-methyls-non-alkyl active group-ammonium halide, and m, n are double alkane
The carbon number of base chain, its value be 14~24, halogen is chlorine or bromine, non-alkyl active group be alkoxy, carbonyl, carboxyl,
One kind in benzyl.
4. the production method of the organic clay of a kind of big interplanar distance according to claim 2, it is characterised in that filtering is
After adding water to stir the product mixed serum for the reaction that organises, common plate and frame filter press, diaphragm filter press, vacuum filtration are moved into
Machine or centrifuge, filter off moisture and soluble ion.
5. the production method of the organic clay of a kind of big interplanar distance according to claim 2, it is characterised in that ageing is
Filter cake after filtering is placed at shady and cool ventilation and stacked 8~48 hours.
6. the production method of the organic clay of a kind of big interplanar distance according to claim 2, it is characterised in that drying is
Product after ageing is dried to moisture content≤3.5% under 100~150 DEG C of environment.
7. the production method of the organic clay of a kind of big interplanar distance according to claim 2, it is characterised in that crushing is
Dried product is ground into by least 80 mesh or average grain diameter≤0.173mm using pulverizer.
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