DE2139952C2 - Process for the production of heavy materials for drilling fluids - Google Patents

Description

is to be made and all drilling 10 μ mentioned at the beginning is not more than 50%. Such a protechnical one Requirements of a weighting device met. duct has roughly the same composition

To this end, the invention is based on a method for gQo / p _Co o

Production of weighting agents for drilling fluids _{00 /} ° ^{2 3} '

through fine processing to less than 2% total sulfur 5 "">

rusted, sulfidic iron ores, neutralization of the 7%

goods dispersed in water, leaching of soluble 2% Pb, Zn

Proportions and subsequent drying of the good. 1.5% AI ₂ O ₃ ,

In the context of the specified working method, there is _{n Q0} / r. «» Camt «* Wp.fM

The process of linking is then that a post-10th

Fluidized bed process of roasted flotalion pyrite and contains about 3.6% water-soluble components, used and to a grain fineness below 75 μ klas- To remove these water-soluble fractions is

is siert, with the grain fraction below 10 μ not flour the rusted flotation pyrite in water from 40 to than 50%; it is preferably no longer 80 ° C. in suspension, the suspension being about 500 g than 30%. Such, according to the fluidized bed process, has 15 solids per liter.

Rusted flotation pyrites have an iron oxide- In general, a treatment time of is sufficient

content (Fe ₂ O ^) of at least 70%. Preferably for about 30 minutes with gentle stirring at Tempewerdeii such preparation products in the inventive ratures of 50 to 70 C. Here, the water-based methods are used, which contain an iron oxide-soluble constituents, e.g. B. the salts have polyvalent content of at least 75% and up to 95%. 20 cations such as calcium, iron, aluminum, zinc and

The total sulfur content of the other in solution. The suspension is filtered off in a roasted flota manner used in known methods; it is expedient to use a rotating pyrite to be at most 1.5%. It is located upstream filter drained and washed with water at 6O ⁰ C, preferably below 1% and is not the Sulfatge'.alt is given to values below 0.1% more than 0.9% in general. It is decreased for the verse according to the invention. After another slurry in drive critical, that a classification for the production of water, the suspension is subjected to a wet classification with a material specific ¹ "grain composition pre-hydrocyclones and we assume a grain size for the according to the invention

Weights to be produced in accordance with the process for 30 ⁵² ° ^μ>

Drilling fluids proven: 11% 20 to 30 μ,

50 to 55% with a particle size of 30 to 75 μ, ^l } JJ? ^bl * ² ° ^μ>

¹ O to 15% with a particle size of 20 to 30 μ, ^{/ o 1S μ} "

10 to 15% with a particle size of 10 to 20 μ, 35 It has also proven to be advantageous that the

20 to 30% with a particle size of up to 10 μ. washed product shows no acidic reaction. the

Filter cake is therefore again in water at 60 ° C

With such a grain composition Hu "Findicken are elutriated and the suspension means of aqueous UEAs Aliav-izcn DZZ Beschwermitte! ', The ammonia adjusted to a pH of 7 to 8 Rinsing liquid and the foaming during the incorporation of 40 After a treatment time of 30 Iviiuutcn ucl 6C ⁰ C prevents the Beschwermittels into the flushing liquid. The solid is separated off with constant stirring

It is for the texture and quality of the loading and washing out. The washed out product will Heavy means without influence, at which point of the Ver then dried to a residual moisture of about 0.4%, The process sequence of the method according to the invention is based on a further embodiment of the invention

Classification is carried out. 45 is the washed out product, which if necessary

A treatment with neutralizing reagents can therefore also be carried out according to the fluidized bed process Roasted flotation pyrite has been subjected directly to the specified, with water-soluble barium compound grain composition brought and then treated the fertilizer. Be with this treatment further treatment. But it can contain salts that are not fully washable and still do A roasted product can also be used because it interferes with the existing solubility in drilling fluids, such as Creativity, as converted into insoluble barium sulfate after roasting flotation calcium sulfate accrues in the fluidized bed, with the classification. This remains in after being washed out again treatment treatment after the washing process and has no after-effects in the weighting agent can be. For example, in a wet part, more influence on the drilling fluid, classification of the washed and resuspended 55 According to a further embodiment of the invention th product by means of hydrocyclones, the invention can remove the water-soluble components according to the grain composition of the weighting agents weighting agents are treated with substances which can be set. Finally, however, one can also influence the surface of the product. Such partial preparation of the roasted product before the substances are z. B. surfactants such as triethynolamine or Process sequence and the final classification 60 means against the loss of fluid in the drilling fluid during or at the end of the process, like sodium carboxymethyl cellulose. The effect be taken. of these additives, which are used, for example, in the re-

Appropriately, a mode of operation has been added for the invention slurry in the washing process Proven method according to the invention, in which, according to the can, consists in the better dispersibility of the Fluidized bed process of roasted flotation gravel with 65 weighting means.

next brought to a residual moisture of about 1% If no wet classification is carried out,

and this material is ground in such a way that classification can also be carried out after the the fineness is below 100 μ and the grain fraction is made under washed-out goods, which

5 6

also with the surface of the product influencing in turn to 500 g solids per liter slurried, substances can be treated. In such a K-lassie- ii.it dilute aqueous ammonia solution a tion is the Restfeuchle of the material under appropriate pH-value of 7 is set to 8, 30 minutes at 60 ° C L ° / ₀ and is about 0.4 ^u / ₀ . stirred and again dehydrated through a rotary filter. The prepared according to the method of the invention and ^{washed with 60 1} C warm water. The filter weighting agent can, for. B. in clay-salt water rinsing cake was used in a drum dryer at 110'C. Such drilling fluids have dried up to a Rcstfeuchte of 0.4 ° / _0th D'eses beieinewipH-Werl of about 11 and a specific material was separated by sieving parts with a weight greater than 1.2 to about the following composition: 75 μ and now had the

". . ίο guided grain size analysis.

inrT ^e " ^Tabeilc 1 ^{also shows the} analysis values and

^{WabSer UMJO} drilling data listed. It shows, that

Bentonite 40 d _cr total sulfur content from 0.9 °, ' _o to 0.2 and the

Carboxymelhy cellulose. 30 water-soluble fraction decreased from 3.6 to 0.0X "',,

Diluent 2 ¹ S was.

Sodium Chloride 30 Example 2

Sodium hydroxide 0.75

By adding 610 g of the weighting agent produced according to the invention, dried and ground according to Example 1, a specific weight of pyrite burn was adjusted to 500 g of solid weight of 1.6 with water. slurried per liter, heated to 60 "C and stirred for 30 ml. the same specific gravity with heavy spar. The suspension was obtained by means of a lathe aiming, 650 g are required. Filters are also dewatered in the same way and rinsing liquids are poured with 60" C warm water with higher specific threaded. wash hten the filter cake was again being made 25 slurried and heated to 6O ⁰ C the erfindungsgemäßc procedure was has advantages \ erdünnte with stirring, ammonia solution up to a pH It allows the use cinc3 Beschwermittels... of 7.5 was added within 10 minutes for drilling fluids with a high specific weight, a separately prepared suspension of 200 g weight, which can be added to 2 liters of water without any noteworthy technical additions of carboxymethanol cellulose and which is more economical 30 and the mixture obtained can be used for 30 minutes at 60 × ge-manner. The special grain structure of the stirs The suspension obtained in this way was dewatered using a rotary filter using the weighting means produced according to the invention and washed at 20 ° C. to prevent it from settling in the drilling fluid and water until the filtrate had a pH of 7.0. The filter cake was as in Example 1 specific gravity at the borehole. 35 dried.

The method according to the invention is shown on the basis of the drilling data in Table 1 on

the following examples explained in more detail. guided. With the addition of CMC, the dispersing

In these examples, there is a swirling ability of the weighting agent in the rinsing liquid

Layering process of rusted flotation pyrite has been improved as follows (grain size analysis see Tabeilc 2).

7ucqmmerT; et7iing and characteristic used: 4 °

Fe ₂ O ₃ ". 80 ° / ₀ At, pie! 3

FeO 2 _^0/0 T _{he nac} | · overall, Example 1, dried, ground and

SiO ₂ 7 _{% / 0} washed pyrite burn was removed with water.

Al ₂ O ₃ 1.5 ° / 45 slurries and to the suspension 500 g BaCl ₂ · 2HoO

p. ₇ ~ \ ₀ , added within 10 minutes. The suspension was

' '"'" then ^{stirred for 30 minutes at 6O 0} C and after

Total S 0.9 / ₀ Example 1 washed, dried and sieved. the

Water-soluble proportions 3.6% / ₀ analysis data are in Table 1, the grain size

pH value 2.9 5 ° analysis listed in Table 2.

Specific gravity 4.5

Example 4

Such a product falls in the production of

Sulfuric acid from SO ₂ , which was burned off by disarming 50 kg of pyrite in a fan mill

Flotation pyrite is ground by the fluidized bed process and the mill application by subsequent is won. Dry sighting on the one listed in Table 2

Grain distribution classified, whereby the coarse part is larger For example 75 μ was returned to the mill.

The main product was carried out according to Example 1

50 kg of the pyrite burn-off described were processed in 60 (analysis data see Table 1, pebbles in a drum dryer for a residual moisture content of 1 ° / ₀ analysis 6- Table 2).
dried. The dried burn-up was carried out in a ball mill filled with steel balls, Example 5, for 2.5 hours
dry ground. This product was made with water

slurried to 500 g of solids per liter and with 65 50 kg of pyrite burn-up were stirred according to Example 1 dry-60 "C for 10 minutes. The suspension obtained is net, ground, washed and neutralized. Which was drained via a rotary filter and 6O ⁰ C filter cake was washed in water to 500 g of solids per warm water. The filter cake was slurried liter and with the help of a hydrocyclone

the coarse fraction greater than 75 μ is separated. The cyclone overflow, i.e. H. Solid with a grain size smaller 75 μ, was filtered and dried according to Example 1. The material showed those listed in Table 1 Analysis data and the particle size analysis given in Table 2.

Example 6

Pyrite burn was slurried with water to 1200 g of solid per liter and 1 hour in a ball mill, filled with steel balls, ground. The mill discharge was classified according to the required grain size composition with the aid of a hydrocyclone

and then dehydrated through a rotary filter and ^{washed with 60 0} C warm water. The filter cake was neutralized with ammonia, washed and dried (analysis data see Table 1, particle size analysis see Table 2).

Example 7

Pyrite burn-up was prepared according to Example 1 and the grain compositions specified there were set. The dry product obtained was mixed with barite, as is used in drilling practice found, mixed dry in a ratio of 1: 1 (analysis data see table 1, grain size analysis see table 2).

Table I.

Barite, the trade

Initial ^{1 2} 3 Examples ⁵ 6th mat. for 83 82 83 82 82 example 1 0.1 0.1 0.1 ^4th 0.1 0.1 to 7 7.6 7.5 7.6 83 7.5 7.5 80 1.5 1.4 1.4 0.1 1.4 1.4 2.0 1.4 1.5 1.4 7-.5 1.4 1.5 7.0 0.2 0.2 0.2 1.5 0.2 0.2 2.0 0.08 0.07 0.06 1.4 0.08 0.10 1.5 0.3 0.4 0.5 0.2 0.4 0.4 0.9 6.8 7.2 6.7 0.09 7.3 6.9 3.6 4.7 4.8 4.7 0.3 4.8 4.8 - 20th 20th 30th 7.2 20th 20th 2.9 28 27 23 4.8 27 28 4.5 27 17th 15th 20th 25th 25th 53 38 33 28 52 52 41 33 29 25th 30th 33 31 24 15th 55 24 24 - 3.8 3.7 3.5 34 3.6 3.5 - 1.1 1.0 1.1 29 1.0 1.0 - 3.5 - 1.0 -

Chemical Analysis
Total iron
Fe ₈ O ₃ , ⁰ I ₀ ....
FeO, ° / ₀

SiO ₂ ,%

Pb, Zn, ⁰ I ₀

Al ₂ O ₃ ,%

Total sulfur

So/

Water-soluble fractions, ° / o · ·· ·

Humidity, ° / o

PH value

specific weight

Abrasion (mg)

Drilling data

Apparent viscosity (cP)

Plastic viscosity (cP)

Yield point (dyn / cm ⁴ )

10 'gel strength

Thixotropic

Water loss

Filter cake thickness (mm)

0.2 0.4 6.9 4.2 40

33

28

69

60

43 3.5 1.0

Note: The drilling data were determined according to “Winnung”, Hanover, June 1968.

42

not detectable 3.7
0.7
0.6

0.10 0.3 7.0 4.4 30th

30th 27 58 45 30th 3.5 1.0 the »guidelines of the working committee in the petroleum industry

table

Grain size analysis
Shares in ° / ₀

1 2 3 Examples 5 6th 7th 50 52 51 ^4th 51 52 50 30 to 75 μ 12th 13th 14th 55 11th 13th 15th 20 to 30 μ 12th 14th 14th 12th 12th 14th 15th 10 to 20 μ 26th 21 21 13th 26th 21 20th 0 to 10 μ 20th

Note: Determination according to Andreasen.

Claims (8)

1 2 to compensate for the formation pressure that occurs. The most important task of the patent claims: The weighting agent is to measure the specific weight of the flushing medium with the least possible use 1. Process for the production of weighted quantities to increase. Such substances, which are suitable as weighting agents for drilling fluids by fouling, must therefore themselves have the highest possible density, roasted to less than 2% total sulfur content. The other sulphidic iron ores, which are important in terms of flushing technology, neutralization of the properties in water during drilling mud, are allowed to use the dispersed material. The leaching of soluble parts of the detrimental substances does not adversely affect the drying of the goods, thereby resulting in ge ke η η- ίο. For example, the weighting means should have little effect on the fact that a flotation pyrite which has been roasted after the fluidized bed viscosity as opposed to carefree flushing is used little. The rinses act and ow! a grain fineness below 75 μ is classified, it is mostly a non-Newtonian liquid, whereby the grain fraction below 10 μ is no more than that which has ring thixotropic effects. A 50 ° / ₀ is. 15 high thi. \ Iropia, combined with a "high flow 2. The method according to claim 1, characterized thereby, makes it more difficult for the flush to be pumped. A is characterized in that a low to a total sulfur content Thixotropic contrast is desired, the less than 1 ° / ₀ abgerösteter Flotationspyrit used sustainability of a rinse for the suspended therein. Allow drilling cuttings. Furthermore, the loading 3. The method according to claims 1 to 2, da- 20 heavy the loss of rinsing liquid and the characterized in that on a grain fineness ingress of rock water on the borehole wall is classified below 75 μ, whereby the grain fraction is so due to the formation of a dense filter clump below 10 μ is not more than 30%. keep it as low as possible. Furthermore, the complaint 4. The method according to claims 1 to 3, there- medium a low abrasion effect in terms of characterized in that the classification to 25 include the wear and tear of the drilling equipment. About it The weighting agent used must not have a grain composition of the rinsing liquid still with the various 50 to 55 _^0/0 30 to 75 μ, enter into rock strata chemical reactions. 10 to 15% 20 to 30 μ, It is known that to meet these requirements 10 to 15% 10 to 20 μ, 3 ° ⁿ isse processed, natural heavy spar with a 20 to 30 ⁰ Z to 10 μ specific gravity of about 4.2 as the weight center! ^{μ is used} for drilling fluids. The processing is made. to products with an equally high specific 5. The method according to claims 1 to 4, because weight is expensive. Substances based on iron oxide, such as characterized in that the classified material is a 35 hematite, magnetite or mill skin scale, with special treatment with the surface of the complaint have weights of up to a maximum of 5.2 as a weighting device is subjected to influencing substances. medium little input into technical practice 6. The method according to claims 1 hh 5. found because they are too expensive compared to heavy spar, characterized in that the classified goods have one and flushing technology Nachieiie, such as liui ». Abrate. ". Treatment with water-soluble barium compounds and a tendency to sedimentation. gen is subjected. After a known suggestion, a complaint 7. The method according to claims 1 to 6, there- fore, for drilling fluids from roasted sulphide, characterized in that the leaching is produced in the case of iron ores (US Pat. No. 2 298 984). Water temperatures of 40 to 8O ⁰ C, preferential The high total sulfur content of the erosion is of to 70 ⁰ C, performed as 50th 45 previously known method makes it necessary this 8. The method according to claims 1 to 7, da- a calcination, in particular a chlorinating one, characterized in that to subject the aqueous roasting at about 1000 ⁰ C using slurries before leaching neutral alkali metal salts. It is also sationsmittel added. required, the water-soluble components in connection Wash out 50 with a wet grind. The previously known method has disadvantages insofar as the Calcination process is expensive and the weighting agent still contains fluctuating proportions of gait and thus the production of a weighting device with equal to -55 moderately high specific gravity in a reproducible manner is not possible. The development of today's drilling technology is approaching The invention relates to a method for ever increasing depths. This is what rinsing fluids are for Production of weighting agents for drilling fluids with specific gravity over 2.0 required. Like that rinsing liquids obtained through the fine processing of roasted sulphidic iron can be processed with Neutralization of the aqueous dispersion of the tetem Naturschwers.pat (specific weight about 4.2) Good, washing out and drying. Lim only obtainable if one accepts other disadvantages previously known method is inventively a takes, such as deterioration of the viscosity of the Bohrnach the fluidized bed process of roasted float rinsing liquid. tion pyrite used, and it wirü a classification 65. The invention is based on the object of a case certain contractions and amounts of heavy medium high, at least 4.7 amount, specially carried out, To provide fish weight for drilling fluids, it is known that flushing fluids at great depths in a technically simple and economical manner