CN116588964A - Barium sulfate and preparation method thereof - Google Patents
Barium sulfate and preparation method thereof Download PDFInfo
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- CN116588964A CN116588964A CN202310409010.XA CN202310409010A CN116588964A CN 116588964 A CN116588964 A CN 116588964A CN 202310409010 A CN202310409010 A CN 202310409010A CN 116588964 A CN116588964 A CN 116588964A
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- barium
- sodium sulfate
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- TZCXTZWJZNENPQ-UHFFFAOYSA-L barium sulfate Chemical compound [Ba+2].[O-]S([O-])(=O)=O TZCXTZWJZNENPQ-UHFFFAOYSA-L 0.000 title claims abstract description 91
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 claims abstract description 110
- 229910052938 sodium sulfate Inorganic materials 0.000 claims abstract description 90
- 235000011152 sodium sulphate Nutrition 0.000 claims abstract description 90
- 239000002002 slurry Substances 0.000 claims abstract description 51
- 229910052788 barium Inorganic materials 0.000 claims abstract description 40
- DSAJWYNOEDNPEQ-UHFFFAOYSA-N barium atom Chemical compound [Ba] DSAJWYNOEDNPEQ-UHFFFAOYSA-N 0.000 claims abstract description 40
- CJDPJFRMHVXWPT-UHFFFAOYSA-N barium sulfide Chemical compound [S-2].[Ba+2] CJDPJFRMHVXWPT-UHFFFAOYSA-N 0.000 claims abstract description 37
- 238000006243 chemical reaction Methods 0.000 claims abstract description 28
- 238000005406 washing Methods 0.000 claims abstract description 18
- 238000001035 drying Methods 0.000 claims abstract description 14
- 239000007788 liquid Substances 0.000 claims abstract description 12
- 239000002245 particle Substances 0.000 claims abstract description 10
- 239000000843 powder Substances 0.000 claims abstract description 9
- 238000000926 separation method Methods 0.000 claims abstract description 9
- 238000003825 pressing Methods 0.000 claims abstract description 6
- 239000007790 solid phase Substances 0.000 claims abstract description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 83
- 238000003756 stirring Methods 0.000 claims description 47
- 238000000034 method Methods 0.000 claims description 27
- 238000001914 filtration Methods 0.000 claims description 24
- 229910052979 sodium sulfide Inorganic materials 0.000 claims description 10
- GRVFOGOEDUUMBP-UHFFFAOYSA-N sodium sulfide (anhydrous) Chemical compound [Na+].[Na+].[S-2] GRVFOGOEDUUMBP-UHFFFAOYSA-N 0.000 claims description 10
- 238000001704 evaporation Methods 0.000 claims description 6
- 239000007791 liquid phase Substances 0.000 claims description 4
- 230000032683 aging Effects 0.000 claims 1
- 238000003786 synthesis reaction Methods 0.000 abstract description 13
- 230000015572 biosynthetic process Effects 0.000 abstract description 12
- 238000009826 distribution Methods 0.000 abstract description 6
- 239000000243 solution Substances 0.000 description 96
- 238000010438 heat treatment Methods 0.000 description 43
- 239000000523 sample Substances 0.000 description 38
- 239000000706 filtrate Substances 0.000 description 29
- 238000005259 measurement Methods 0.000 description 23
- 239000000047 product Substances 0.000 description 23
- 238000003860 storage Methods 0.000 description 18
- 238000012360 testing method Methods 0.000 description 15
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 13
- 239000008399 tap water Substances 0.000 description 9
- 235000020679 tap water Nutrition 0.000 description 9
- 238000005303 weighing Methods 0.000 description 9
- 239000010963 304 stainless steel Substances 0.000 description 8
- 229910000589 SAE 304 stainless steel Inorganic materials 0.000 description 8
- 238000004458 analytical method Methods 0.000 description 8
- ZCYVEMRRCGMTRW-UHFFFAOYSA-N 7553-56-2 Chemical compound [I] ZCYVEMRRCGMTRW-UHFFFAOYSA-N 0.000 description 7
- 239000003153 chemical reaction reagent Substances 0.000 description 7
- 239000011630 iodine Substances 0.000 description 7
- 229910052740 iodine Inorganic materials 0.000 description 7
- 238000004448 titration Methods 0.000 description 7
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 6
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 6
- 239000011521 glass Substances 0.000 description 6
- 229910052742 iron Inorganic materials 0.000 description 6
- AKHNMLFCWUSKQB-UHFFFAOYSA-L sodium thiosulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=S AKHNMLFCWUSKQB-UHFFFAOYSA-L 0.000 description 6
- 235000019345 sodium thiosulphate Nutrition 0.000 description 6
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 5
- 238000004364 calculation method Methods 0.000 description 5
- 239000003921 oil Substances 0.000 description 5
- 235000019198 oils Nutrition 0.000 description 5
- 239000002994 raw material Substances 0.000 description 5
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 4
- 235000021388 linseed oil Nutrition 0.000 description 4
- 239000000944 linseed oil Substances 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 239000012528 membrane Substances 0.000 description 4
- 239000011734 sodium Substances 0.000 description 4
- 239000012086 standard solution Substances 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 239000000725 suspension Substances 0.000 description 4
- 238000003556 assay Methods 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 238000001816 cooling Methods 0.000 description 3
- 238000002386 leaching Methods 0.000 description 3
- 239000010446 mirabilite Substances 0.000 description 3
- 229910052573 porcelain Inorganic materials 0.000 description 3
- 239000002244 precipitate Substances 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 229920002472 Starch Polymers 0.000 description 2
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 description 2
- 238000002835 absorbance Methods 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 238000009835 boiling Methods 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 239000002274 desiccant Substances 0.000 description 2
- 239000012153 distilled water Substances 0.000 description 2
- 230000008020 evaporation Effects 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 230000003287 optical effect Effects 0.000 description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 2
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 description 2
- GCLGEJMYGQKIIW-UHFFFAOYSA-H sodium hexametaphosphate Chemical compound [Na]OP1(=O)OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])O1 GCLGEJMYGQKIIW-UHFFFAOYSA-H 0.000 description 2
- 235000019982 sodium hexametaphosphate Nutrition 0.000 description 2
- 239000008107 starch Substances 0.000 description 2
- 235000019698 starch Nutrition 0.000 description 2
- 239000006228 supernatant Substances 0.000 description 2
- 238000010998 test method Methods 0.000 description 2
- 239000012085 test solution Substances 0.000 description 2
- 239000001577 tetrasodium phosphonato phosphate Substances 0.000 description 2
- 239000003039 volatile agent Substances 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 241000195493 Cryptophyta Species 0.000 description 1
- 241001411320 Eriogonum inflatum Species 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 239000003929 acidic solution Substances 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 238000004380 ashing Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000012496 blank sample Substances 0.000 description 1
- 239000012490 blank solution Substances 0.000 description 1
- 230000001680 brushing effect Effects 0.000 description 1
- 239000001913 cellulose Substances 0.000 description 1
- 229920002678 cellulose Polymers 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000008395 clarifying agent Substances 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000008367 deionised water Chemical group 0.000 description 1
- 229910021641 deionized water Chemical group 0.000 description 1
- 210000003298 dental enamel Anatomy 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000007865 diluting Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 239000012847 fine chemical Substances 0.000 description 1
- 238000011010 flushing procedure Methods 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 238000001033 granulometry Methods 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 239000005337 ground glass Substances 0.000 description 1
- 239000010460 hemp oil Substances 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000003760 magnetic stirring Methods 0.000 description 1
- 239000004579 marble Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 230000009965 odorless effect Effects 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 230000002285 radioactive effect Effects 0.000 description 1
- 238000010992 reflux Methods 0.000 description 1
- 239000005060 rubber Substances 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 238000004062 sedimentation Methods 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 229910001961 silver nitrate Inorganic materials 0.000 description 1
- 238000004513 sizing Methods 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 230000000087 stabilizing effect Effects 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000000967 suction filtration Methods 0.000 description 1
- 239000004753 textile Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F11/00—Compounds of calcium, strontium, or barium
- C01F11/46—Sulfates
- C01F11/462—Sulfates of Sr or Ba
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B17/00—Sulfur; Compounds thereof
- C01B17/22—Alkali metal sulfides or polysulfides
- C01B17/40—Making shaped products, e.g. granules
-
- 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
- C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/60—Optical properties, e.g. expressed in CIELAB-values
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Abstract
The invention provides a preparation method of barium sulfate, which comprises the following steps: (1) Respectively carrying out filter pressing on the crude barium sulfide solution and the crude sodium sulfate solution to obtain a barium sulfide solution and a sodium sulfate solution; (2) Feeding a barium sulfide solution and a sodium sulfate solution into a microcavity reactor for reaction to obtain barium slurry; (3) The barium slurry automatically flows into a curing tank to carry out curing reaction, so as to obtain product slurry; (4) Washing and drying a solid phase obtained by solid-liquid separation of the product slurry to obtain powder barium sulfate. The invention also provides barium sulfate with the particle diameter D50 of 0.30-0.80 mu m and the whiteness of more than 99. The preparation method of the invention has low cost, high synthesis efficiency and yield, and the barium sulfate product has high quality, uniform particle size distribution, high whiteness and no smell.
Description
Technical Field
The invention belongs to the field of inorganic fine chemical industry, and particularly relates to barium sulfate and a preparation method thereof.
Background
The barium sulfate is white amorphous powder in appearance, has the advantages of strong chemical inertia, good stability, acid and alkali resistance, moderate hardness, high whiteness, high gloss, capability of absorbing harmful x-rays, gamma-rays and the like, and is widely used as a material with environmental protection function for various coatings, printing ink, plastic rubber and raw materials or filling agents of storage batteries; surface coating agents for printing paper and copper plate paper, sizing agents for textile industry; can be used as clarifying agent in glass products, and has the functions of defoaming and increasing gloss. Can also be used as a protective wall material for preventing radioactive rays, and is also used in industries such as porcelain, enamel, fuel and the like. At present, the barium sulfate produced by the process has the defects of uneven particle size distribution, low whiteness, heavy smell and the like, and the conventional mirabilite method is adopted in production, so that the existing market demands cannot be met.
Therefore, there is a need in the art for a low cost, uniform particle size distribution, high whiteness, odorless process.
Disclosure of Invention
In view of the above problems, an object of the present invention is to provide a barium sulfate and a method for producing the same, so as to obtain barium sulfate having a uniform particle size distribution, a high whiteness, and no odor.
In one aspect, the invention provides a method for preparing barium sulfate, comprising the following steps:
(1) Respectively carrying out filter pressing on the crude barium sulfide solution and the crude sodium sulfate solution to obtain a barium sulfide solution and a sodium sulfate solution;
(2) Feeding a barium sulfide solution and a sodium sulfate solution into a microcavity reactor for reaction to obtain barium slurry;
(3) The barium slurry automatically flows into a curing tank to carry out curing reaction, so as to obtain product slurry;
(4) Washing and drying a solid phase obtained by solid-liquid separation of the product slurry to obtain powder barium sulfate.
Optionally, in the step (4), the liquid phase obtained by solid-liquid separation of the product slurry is evaporated and flaked to obtain sodium sulfide.
Alternatively, the evaporated condensate in step (4) is used to wash the solid phase of the product slurry obtained by solid-liquid separation, and the resulting wash water is used in step (1) to prepare a crude barium sulfide solution and a crude sodium sulfate solution.
Optionally, in step (1), the concentration of the crude barium sulfide solution is 10% -15%, the concentration of the crude sodium sulfate solution is 25% -30%, and the press filtration is performed at 60 ℃ -70 ℃.
Optionally, in step (2), the barium sulfide solution is fed into the microcavity reactor at a rate of 12m 3 /h～17m 3 The rate of sodium sulfate solution input into the microcavity reactor was 2m 3 /h～7m 3 And/h, the stirring rotating speed of the microcavity reactor is 495 r/min-505 r/min.
Optionally, in step (3), the curing reaction includes adjusting the reaction endpoint by feeding sodium sulfate into the barium slurry to cause the barium slurry to be slightly nitrosated.
On the other hand, the invention provides the barium sulfate which is prepared by adopting the preparation method, wherein the particle diameter D50 of the barium sulfate is 0.30-0.80 mu m, and the whiteness is more than 99.
According to the technical scheme, the barium sulfate and the preparation method thereof have at least the following beneficial effects:
(1) The preparation method of barium sulfate of the invention, calcine barium sulfide solution and anhydrous sodium sulfate (anhydrous sodium sulfate) raw materials leached with the heavy-duty ore, get barium sulfate crystal seed after the reaction of microcavity reactor, get barium sulfate slurry that distributes evenly after adjusting the end point, barium slurry, get powder barium sulfate products through solid-liquid separation, washing, drying, the sodium sulfide solution produced by synthesis is evaporated, flaked to get the flaky sodium sulfide products;
(2) According to the preparation method of the barium sulfate, mechanical impurities in raw materials of barium sulfide and sodium sulfate are removed by filter pressing;
(3) According to the preparation method of the barium sulfate, equipment made of the stainless steel with the thickness of 304 and above is adopted, so that the iron content in the product is prevented from being higher due to corrosion of the equipment, and the quality of the product is ensured;
(4) According to the preparation method of the barium sulfate, the sodium sulfide solution is evaporated and concentrated to produce the sodium sulfide product, the condensate is used for washing the barium sulfate, and the washing water is used for preparing the sodium sulfate solution and leaching yellow water, so that zero emission of process water is truly realized, and environmental pollution is avoided;
(5) The particle size D50 of the barium sulfate obtained by the preparation method of the barium sulfate can be controlled between 0.30 and 0.8 mu m, the particle size distribution is uniform, the whiteness is more than 99, and the barium sulfate has no smell. Therefore, the product quality of the barium sulfate is improved, the application of the downstream fine industry is met, and the economic value is better.
Drawings
Various other advantages and benefits will become apparent to those of ordinary skill in the art upon reading the following detailed description of the preferred embodiments. The drawings are only for purposes of illustrating the preferred embodiments and are not to be construed as limiting the invention. In the drawings:
fig. 1 is a process flow diagram of a barium sulfate preparation method of the present invention.
Detailed Description
The present invention will be described in detail with reference to the following embodiments for a full understanding of the objects, features, and effects of the present invention. The process of the present invention is carried out by methods or apparatus conventional in the art, except as described below. The following terms have the meanings commonly understood by those skilled in the art unless otherwise indicated.
In order to solve the quality problem caused by the barium sulfate produced by the traditional mirabilite method, the inventor of the invention develops a new process, and provides a preparation method of the barium sulfate, which can improve the synthesis efficiency and yield, stabilize and improve the product quality and meet the requirements of customers.
As shown in fig. 1, the preparation method of the barium sulfate of the present invention comprises:
(1) Raw material preparation
Collecting barium sulfide solution (yellow water) with concentration of 10% -15% from an leaching workshop, press-filtering to obtain clarified barium sulfide solution for standby, preparing sodium sulfate solution with concentration of 25% -30%, press-filtering to obtain clarified sodium sulfate solution for standby, heating and preserving raw materials in the whole process, and controlling the temperature at 65+/-5 ℃.
(2) Microcavity reactor synthesis reaction
The barium sulfide solution and the sodium sulfate solution are used for a certain flow rate, preferablyThe barium sulfide solution is 12m 3 /h～17m 3 Sodium sulfate solution of 2m 3 /h～7m 3 And (h) simultaneously entering a microcavity reactor for reaction, wherein the stirring rotating speed of the microcavity reactor is controlled to be 500+/-5 r/min; wherein, the reaction equation for producing barium sulfate by mirabilite method is:
Na 2 SO 4 +BaS＝BaSO4↓+Na 2 S
the microcavity reactor can be an existing microcavity reactor, and the invention does not have special requirements.
(3) Curing reaction
The reacted barium slurry automatically flows into a curing tank for storage, and after the barium slurry is positioned in the curing tank to a certain scale, the synthesis is stopped; after the barium slurry is stored in the curing tank, the reaction end point is adjusted to make the barium slurry slightly oversterite (namely, sodium sulfate is excessive by 2% or less according to the stoichiometric ratio), and stirring is continued, for example, 4 hours to finish the reaction. The reaction end point can be adjusted by inputting sodium sulfate solution.
(4) The barium slurry after the reaction is subjected to solid-liquid separation, and the solid-phase barium sulfate is washed and dried to obtain a powder barium sulfate product; evaporating and flaking the liquid-phase sodium sulfide solution to obtain a sodium sulfide product.
(5) The condensate of the evaporator adopted by the evaporation of liquid-phase sodium sulfide is used for washing barium sulfate, and the washing water is finally used for preparing anhydrous sodium sulfate and leaching yellow water, so that the process water is discharged in a zero way in the whole process.
Example 1
Collecting 100m of 12.5% barium sulfide solution 3 Heating and preserving the temperature in a storage tank to 60-70 ℃, press-filtering, heating and preserving the temperature of filtrate barium sulfide solution to 62 ℃, and adding 8m in a sodium sulfate dissolving tank 3 Adding tap water into 3t anhydrous sodium sulfate under heating and stirring, heating and maintaining the temperature at 60-70deg.C, press filtering after anhydrous sodium sulfate is completely dissolved, storing filtrate in sodium sulfate solution storage tank, heating and maintaining the temperature at 62 deg.C, and repeating for 3 times. Starting a microcavity reactor for stirring, controlling the stirring rotating speed to be 500r/min, starting a yellow water valve of the reactor, starting a yellow water pump to adjust a yellow water flowmeter to enable the yellow water flow to be 15m 3 And/h, restarting a sodium sulfate valve of the reactor, and starting a sodium sulfate pump to regulate sulfuric acidThe sodium solution flowmeter enables the flow rate of the sodium sulfate solution to be 5m 3 And (3) starting synthesis, namely automatically flowing barium slurry into a curing tank through a reactor, stirring and storing, closing a yellow water valve and a sodium sulfate valve after the micro-reactor reacts for 4 hours, stopping the reaction, continuously opening a sodium sulfate solution valve, and continuously stirring for 4 hours after the barium slurry in the curing tank is slightly over-nitrated. And separating, washing and drying the barium slurry overnight to obtain 10.3 tons of products. The equipment used is 304 stainless steel.
Example 2
Collecting 100m of 12.5% barium sulfide solution 3 Heating and preserving the temperature in a storage tank to 60-70 ℃, press-filtering, heating and preserving the temperature of filtrate barium sulfide solution to 63 ℃, and adding 8m in a sodium sulfate dissolving tank 3 Adding tap water into 3t anhydrous sodium sulfate under heating and stirring, heating and maintaining the temperature at 60-70deg.C, press filtering after anhydrous sodium sulfate is completely dissolved, storing filtrate in sodium sulfate solution storage tank, heating and maintaining the temperature at 69 deg.C, and repeating for 3 times. Starting a microcavity reactor for stirring, controlling the stirring rotating speed to be 500r/min, starting a yellow water valve of the reactor, starting a yellow water pump to adjust a yellow water flowmeter to enable the yellow water flow to be 15m 3 And/h, restarting a sodium sulfate valve of the reactor, and starting a sodium sulfate pump to adjust a sodium sulfate solution flowmeter to enable the flow rate of the sodium sulfate solution to be 5m 3 And (3) starting synthesis, namely automatically flowing barium slurry into a curing tank through a reactor, stirring and storing, closing a yellow water valve and a sodium sulfate valve after the micro-reactor reacts for 4 hours, stopping the reaction, continuously opening a sodium sulfate solution valve, and continuously stirring for 4 hours after the barium slurry in the curing tank is slightly over-nitrated. And separating, washing and drying the barium slurry overnight to obtain 10.3 tons of products. The equipment used is 304 stainless steel.
Example 3
Collecting 100m of 12.3% barium sulfide solution 3 Heating and preserving the temperature in a storage tank to 60-70 ℃, press-filtering, heating and preserving the temperature of filtrate barium sulfide solution to 60 ℃, and adding 8m in a sodium sulfate dissolving tank 3 Adding tap water under heating and stirring to 3t sodium sulfate, heating and maintaining the temperature at 60-70deg.C, press filtering after sodium sulfate is completely dissolved, and storing filtrate in sodium sulfate solution storage tankThe heating and heat preservation temperature is 68 ℃, and the process is repeated for 3 times. Starting a microcavity reactor for stirring, controlling the stirring rotating speed to be 500r/min, starting a yellow water valve of the reactor, starting a yellow water pump to adjust a yellow water flowmeter to enable the yellow water flow to be 15m 3 And/h, restarting a sodium sulfate valve of the reactor, and starting a sodium sulfate pump to adjust a sodium sulfate solution flowmeter to enable the flow rate of the sodium sulfate solution to be 5m 3 And (3) starting synthesis, namely automatically flowing barium slurry into a curing tank through a reactor, stirring and storing, closing a yellow water valve and a sodium sulfate valve after the micro-reactor reacts for 4 hours, stopping the reaction, continuously opening a sodium sulfate solution valve, and continuously stirring for 4 hours after the barium slurry in the curing tank is slightly over-nitrated. The barium slurry is separated, washed and dried overnight to obtain 10.1 tons of product. The equipment used is 304 stainless steel.
Example 4
Collecting 100m of 12% barium sulfide solution 3 Heating and preserving the temperature in a storage tank to 60-70 ℃, press-filtering, heating and preserving the temperature of filtrate barium sulfide solution to 69 ℃, and adding 8m in a sodium sulfate dissolving tank 3 Adding tap water into 3t anhydrous sodium sulfate under heating and stirring, heating and maintaining the temperature at 60-70deg.C, press filtering after anhydrous sodium sulfate is completely dissolved, storing filtrate in sodium sulfate solution storage tank, heating and maintaining the temperature at 60deg.C, and repeating for 3 times. Starting a microcavity reactor for stirring, controlling the stirring rotating speed to be 500r/min, starting a yellow water valve of the reactor, starting a yellow water pump to adjust a yellow water flowmeter to enable the yellow water flow to be 15m 3 And/h, restarting a sodium sulfate valve of the reactor, and starting a sodium sulfate pump to adjust a sodium sulfate solution flowmeter to enable the flow rate of the sodium sulfate solution to be 5m 3 And (3) starting synthesis, namely automatically flowing barium slurry into a curing tank through a reactor, stirring and storing, closing a yellow water valve and a sodium sulfate valve after the micro-reactor reacts for 4 hours, stopping the reaction, continuously opening a sodium sulfate solution valve, and continuously stirring for 4 hours after the barium slurry in the curing tank is slightly over-nitrated. The barium slurry is separated, washed and dried overnight to obtain 9.9 tons of products. The equipment used is 304 stainless steel.
Example 5
Collecting 100m of 12% barium sulfide solution 3 Heating and preserving heat in a storage tank to maintain the temperature at 60-70 ℃,after filter pressing, the filtrate barium sulfide solution is heated to 67 ℃ and added with 8m in a sodium sulfate solution tank 3 Adding tap water into 3t anhydrous sodium sulfate under heating and stirring, heating and maintaining the temperature at 60-70deg.C, press filtering after anhydrous sodium sulfate is completely dissolved, storing filtrate in sodium sulfate solution storage tank, heating and maintaining the temperature at 63deg.C, and repeating for 3 times. Starting a microcavity reactor for stirring, controlling the stirring rotating speed to be 500r/min, starting a yellow water valve of the reactor, starting a yellow water pump to adjust a yellow water flowmeter to enable the yellow water flow to be 15m 3 And/h, restarting a sodium sulfate valve of the reactor, and starting a sodium sulfate pump to adjust a sodium sulfate solution flowmeter to enable the flow rate of the sodium sulfate solution to be 5m 3 And (3) starting synthesis, namely automatically flowing barium slurry into a curing tank through a reactor, stirring and storing, closing a yellow water valve and a sodium sulfate valve after the micro-reactor reacts for 4 hours, stopping the reaction, continuously opening a sodium sulfate solution valve, and continuously stirring for 4 hours after the barium slurry in the curing tank is slightly over-nitrated. The barium slurry is separated, washed and dried overnight to obtain 9.9 tons of products. The equipment used is 304 stainless steel.
Example 6
Collecting 100m of 12.8% barium sulfide solution 3 Heating and preserving the temperature in a storage tank to 60-70 ℃, press-filtering, heating and preserving the temperature of filtrate barium sulfide solution to 66 ℃, and adding 8m in a sodium sulfate dissolving tank 3 Adding tap water into 3t anhydrous sodium sulfate under heating and stirring, heating and maintaining the temperature at 60-70deg.C, press filtering after anhydrous sodium sulfate is completely dissolved, storing filtrate in sodium sulfate solution storage tank, heating and maintaining the temperature at 66 deg.C, and repeating for 3 times. Starting a microcavity reactor for stirring, controlling the stirring rotating speed to be 500r/min, starting a yellow water valve of the reactor, starting a yellow water pump to adjust a yellow water flowmeter to enable the yellow water flow to be 15m 3 And/h, restarting a sodium sulfate valve of the reactor, and starting a sodium sulfate pump to adjust a sodium sulfate solution flowmeter to enable the flow rate of the sodium sulfate solution to be 5m 3 And (3) starting synthesis, namely automatically flowing barium slurry into a curing tank through a reactor, stirring and storing, closing a yellow water valve and a sodium sulfate valve after the micro-reactor reacts for 4 hours, stopping the reaction, continuously opening a sodium sulfate solution valve, and continuously stirring for 4 hours after the barium slurry in the curing tank is slightly over-nitrated. Barium (Ba)The pulp is separated, washed and dried overnight to obtain 10.5 tons of product. The equipment used is 304 stainless steel.
Example 7
Collecting 100m of 12.8% barium sulfide solution 3 Heating and preserving the temperature in a storage tank to 60-70 ℃, press-filtering, heating and preserving the temperature of filtrate barium sulfide solution to 65 ℃, and adding 8m in a sodium sulfate dissolving tank 3 Adding tap water into 3t anhydrous sodium sulfate under heating and stirring, heating and maintaining the temperature at 60-70deg.C, press filtering after anhydrous sodium sulfate is completely dissolved, storing filtrate in sodium sulfate solution storage tank, heating and maintaining the temperature at 65deg.C, and repeating for 3 times. Starting a microcavity reactor for stirring, controlling the stirring rotating speed to be 500r/min, starting a yellow water valve of the reactor, starting a yellow water pump to adjust a yellow water flowmeter to enable the yellow water flow to be 15m 3 And/h, restarting a sodium sulfate valve of the reactor, starting a sodium sulfate pump to adjust a sodium sulfate solution flowmeter to enable the flow rate of the sodium sulfate solution to be 7m 3 And (3) starting synthesis, namely automatically flowing barium slurry into a curing tank through a reactor, stirring and storing, closing a yellow water valve and a sodium sulfate valve after the micro-reactor reacts for 4 hours, stopping the reaction, continuously opening a sodium sulfate solution valve, and continuously stirring for 4 hours after the barium slurry in the curing tank is slightly over-nitrated. The barium slurry is separated, washed and dried overnight to obtain 10.5 tons of product. The equipment used is 304 stainless steel.
Example 8
Collecting 100m of 12.5% barium sulfide solution 3 Heating and preserving the temperature in a storage tank to 60-70 ℃, press-filtering, heating and preserving the temperature of filtrate barium sulfide solution to 64 ℃, and adding 8m in a sodium sulfate dissolving tank 3 Adding tap water into 3t anhydrous sodium sulfate under heating and stirring, heating and maintaining the temperature at 60-70deg.C, press filtering after anhydrous sodium sulfate is completely dissolved, storing filtrate in sodium sulfate solution storage tank, heating and maintaining the temperature at 67 deg.C, and repeating for 3 times. Starting a microcavity reactor for stirring, controlling the stirring rotating speed to be 500r/min, starting a yellow water valve of the reactor, starting a yellow water pump to adjust a yellow water flowmeter to enable the yellow water flow to be 15m 3 And/h, restarting a sodium sulfate valve of the reactor, and starting a sodium sulfate pump to adjust a sodium sulfate solution flowmeter to enable the flow rate of the sodium sulfate solution to be 8m 3 And (3) starting synthesis, namely automatically flowing barium slurry into a curing tank through a reactor, stirring and storing, closing a yellow water valve and a sodium sulfate valve after the micro-reactor reacts for 4 hours, stopping the reaction, continuously opening a sodium sulfate solution valve, and continuously stirring for 4 hours after the barium slurry in the curing tank is slightly over-nitrated. And separating, washing and drying the barium slurry overnight to obtain 10.3 tons of products. The equipment used is 304 stainless steel.
Comparative example 1
Comparative example 1 differs from example 1 only in that:
the curing reaction adopts sedimentation curing.
Barium sulfate testing method
1. Test method
1.1 appearance discrimination
The appearance was visually determined under natural light.
1.2 determination of barium sulfate content
1.2.1 reagents
1.2.1.1 sulfuric acid solution: 1+15;
1.2.1.2 hydrochloric acid solution: 1+1;
1.2.1.3 silver nitrate solution: 20g/L
1.2.2 instruments and devices
1.2.2.1 electronic analytical balance;
1.2.2.2 high temperature electric furnaces: the temperature can be controlled to be 800+/-20 DEG C
1.2.3 analytical procedure
About 0.5g of the dried sample was weighed to the nearest 0.0002g, placed in a 400mL beaker, 250mL of water, 5mL of hydrochloric acid solution were added, the solution was heated to boiling, 5mL of hot sulfuric acid solution was added at a uniform rate with stirring, the dish was covered, and the beaker was placed on a boiling water bath and held for 2 hours. The precipitate was filtered through a slow quantitative filter paper and washed with hot water until free of chloride (test methods are as before). Placing the precipitate and filter paper into a porcelain crucible which is burnt to constant quality, drying, ashing, and burning to constant quality in a high-temperature furnace.
1.2.4 results calculation
The content of barium sulfate is calculated as mass fraction W1 of barium sulfate (BaSO 4), and the numerical value is expressed in%, calculated as formula (1):
wherein:
m 1-the mass of the precipitate in grams (g);
m-the mass of the sample in grams (g).
Taking the arithmetic average value of the parallel measurement results as the measurement result, wherein the absolute difference value of the two parallel measurement results is not more than 0.2%.
1.3 Determination of volatiles at 105℃
1.3.1 instruments
1.3.1.1 weighing bottle: and (3) a flat shape.
1.3.1.2 oven: can be maintained at 105+/-2 ℃.
1.3.1.3 balance: to 1mg or more.
1.3.1.4 dryer: an effective desiccant is filled in the air conditioner.
1.3.2 Experimental procedure
1.3.2.1 samples
The lid of the weighing flask was opened, placed in an oven at 105.+ -. 2 ℃ and heated for 2h, placed in a desiccator and cooled. The lid was closed and weighed to the nearest 1mg.
A10 g sample layer was evenly spread on the bottom of the weighing flask, covered with a lid and weighed to the nearest 1mg.
1.3.2.2 assay
The lid was removed and the weighing flask was placed in an oven at 105.+ -. 2 ℃ and heated for at least 1h. Cooled in a dryer. The lid was closed and weighed to the nearest 1mg. And heating again for at least 30min, and cooling in a dryer. The lid was closed and re-weighed to the nearest 1mg. The operation was repeated until the difference in continuous weighing did not exceed 5mg. A lower weighing value was recorded.
1.3.3 representation of results
The volatiles (w 2) at 105℃in mass percent are calculated according to formula (2):
wherein: m 1-mass of sample and weighing bottle before drying, g
m 2-mass of dried sample and weighing bottle, g
m-mass of sample, g
1.3.4 allowable difference
Taking the arithmetic average value of the parallel measurement results as the measurement result, wherein the absolute difference value of the two parallel measurement results is not more than 0.02%.
1.4 determination of the Water-soluble content
1.4.1 reagents
Water: fresh secondary distilled water or deionized water, and the PH is 6-7. Other types of water may be used only when the parties agree.
1.4.2 instruments
1.4.2.1 Single Scale volumetric flask: with a volume of 250mL.
1.4.2.2 membrane filter.
Note 1: other types of filters may be used when the parties agree.
2: when a clear and transparent filtrate is obtained with a slow filter paper, a slow filter paper may also be used for filtration.
3: mixed cellulose microporous filter membranes suitable for use in aqueous systems can be used, and filter membranes of other materials can be used if applicable.
1.4.2.3 evaporating dish: flat bottom, glass, platinum, glazed porcelain or silica, and drying to constant weight.
1.4.2.4 water bath evaporator.
1.4.2.5 oven: can maintain the temperature (105+/-2 ℃).
1.4.2.6 balance: the precision was 0.001g.
1.4.2.7 dryer: and an effective desiccant is contained in the container.
1.4.3 steps
10g (to the nearest 0.01 g) of the sample (m 0) are weighed into a beaker, 200mL of water are added and stirred, and the suspension is boiled for 5min. The suspension was rapidly cooled to room temperature, transferred to a 250mL volumetric flask, diluted to the scale with water, shaken with tumbling to achieve thorough mixing, immediately filtered with a membrane filter, the filtrate returned to the filter until the filtrate was clear, the filtration was difficult to perform centrifugation, 100mL of the completely clear filtrate or the centrifugate was removed in a pre-desiccated algae and weighed evaporation pan, and then evaporated to dryness on a water bath evaporator.
Drying in an oven at 105+ -2deg.C, evaporating the residue in a dish, weighing (accurate to 1 mg) after cooling in a dryer, repeating heating and cooling until the values of the water-soluble substances are different by not more than 10% of the final values, heating for at least 30min, recording the residue mass (m 1), and calculating the water-soluble substances with the lower value of the final two weighed values.
Representation of 5.6.7 results
The mass fraction of the water-soluble substance (heat extraction method) w3 is calculated by a formula (3):
wherein:
m 0-sample mass in grams (g);
m 1-mass of residue in g.
Results are reported to 1-bit decimal.
1.5 determination of iron content
1.5.1 method summary
Like GB/T3049-2006 chapter 3.
1.5.2 reagents
Like GB/T3049-2006 chapter 4.
1.5.3 instruments, apparatus
A spectrophotometer with a cuvette with an optical path of 4 cm.
1.5.4 analytical procedure
Drawing of 1.5.4.1 working curve
According to the specification of 6.3 in GB/T3049-2006, a cuvette with an optical path of 4cm and the corresponding dosage of the iron standard solution are used to draw a working curve.
1.5.4.2 assay
About 10g of the sample was weighed to the nearest 0.01g, placed in a 200mL beaker, 100mL of water and 10mL of (1+1) hydrochloric acid solution were added, boiled for 10min with stirring, and cooled. All were transferred to 250mL volumetric flasks, diluted to scale with water and shaken well. Dry filtration, discard the initial 20mL filtrate, retain filtrate.
25mL of the filtrate was pipetted into a 100mL volumetric flask and the operation was started by adding water to about 60mL … … "as necessary, as described below in GB/T3049-2006 at 6.4. The blank solution was also treated.
1.5.5 results calculation
The iron content is expressed in% by mass fraction w4 of iron (Fe), calculated according to formula (4):
wherein:
m 1-a value of the mass of iron in milligrams (mg) from the working curve based on the measured absorbance of the test solution;
m 0-a value of the mass of iron in milligrams (mg) from the working curve based on the measured absorbance of the blank test solution;
m-the mass of the sample in grams (g).
The arithmetic average of the parallel measurement results is taken as the measurement result, and the absolute value of the two parallel measurement results is not more than 0.0005%.
1.6 measurement of whiteness
1.6.1 method summary
The sample was made into a white board by a presser, and the whiteness value was measured on whiteness compared with a standard white board.
1.6.2 instruments, apparatus
1.6.2.1 whiteness guide: as specified in GB/T5950-1996 chapter 5.
1.6.2.2 standard white board: as specified in GB/T5950-1996 chapter 6.
1.6.3 analytical procedure
A certain amount of sample is taken and placed in a sample pressing device, and the sample is pressed into a sample plate with a flat surface, no texture, no blemish and no stain. Each batch of product was pressed with 3 sample plates.
Preheating the stabilizing instrument according to the use instruction of the instrument, zeroing and operating the standard whiteboard adjusting instrument. The whiteness of the sample is measured by placing the sample on an instrument.
1.6.4 results calculation
Taking the arithmetic average value of the parallel measurement results as the measurement result, wherein the absolute difference value of the two parallel measurement results is not more than 1.0.
1.7 measurement of oil absorption
1.7.1 method summary
The sample absorbs refined pressed hemp seed oil under a specified condition.
1.7.2 reagents and materials
1.7.2.1 refined linseed oil having an acid value of 5.0 to 7.0mgKOH/g
1.7.3 instruments and apparatus
1.7.3.1 plates: ground glass or marble, and has a size of 300mm×400mm or more.
1.7.3.2 knife adjustment: the steel hammer-shaped knife body is 140-150 mm long, 20-25 mm at the widest part and not less than 12.5mm at the narrowest part.
1.7.3.3 burette: capacity 10mL, indexing value 0.05mL.
1.7.4 analytical procedure
About 10g of sample is weighed, the sample is accurately positioned to 0.01g, the sample is placed on a flat plate, the linseed oil is dripped into a dripping bottle with known mass and containing the linseed oil, 4 to 5 drops are added at a time, grinding is carried out continuously by a cutter after the oil is added each time, and the sample is added dropwise at the near-end point. However, when the last drop is added, the sample is wetted by the oil and forms a whole mass, and the sample is not cracked or broken when being spread, and can be adhered to a flat plate to form the end point. All operations should be completed within 20 min-25 min, and finally the dropper bottle is weighed.
1.7.5 results calculation
Oil absorption is measured as W5. The values are expressed as the mass of oil absorbed per 100g of sample and are calculated according to formula (5):
wherein:
m 1-a value of the mass of the consumed refined linseed oil in grams (g);
m is the value of the sample mass, and the unit is gram (g).
Taking the arithmetic average value of the parallel measurement results as the measurement result, wherein the absolute difference value of the two parallel measurement results is not more than 1.0g/100g.
1.8 determination of the pH
1.8.2 instruments
1.8.2.1PH measuring device, capable of measuring 0.1 units, is calibrated with a buffer of known pH at the test temperature.
1.8.2.2 balance to an accuracy of 0.01g or more.
1.8.3 Experimental procedure
10g of the sample was weighed to the nearest 0.01g, placed in a 250mL beaker, 10% suspension was prepared with boiled distilled water, stirred for 5 minutes with magnetic stirring, filtered, and the supernatant was cooled and measured with a pH measuring device.
1.8.4 the results show that
The average of the two measurements was calculated to the nearest 0.1 unit.
1.9 determination of fineness
1.9.1 method summary
The sample is dispersed by water, poured into a sieve, repeatedly washed by water until washing liquid is clear, and the oversize is dried and weighed.
1.9.2 instrument and apparatus
1.9.2.1 electrothermal constant temperature drying oven: the temperature can be controlled to be 105+/-2 ℃;
1.9.2.2 experimental screen: r20/3 series, phi 200X 50-0.045/0.032 GB/T6003.1-1997;
1.9.2.3 glass sand core crucible: the aperture is 16 um-40 um;
1.9.2.4 soft brush
1.9.3 analytical procedure
About 200g of the sample was weighed to the nearest 0.1g and placed in an 800mL beaker, and a proper amount of water (typically 500 mL-600 mL) was added first, followed by stirring with a rubber-tipped glass rod to aid in its dispersion. The dispersed suspension was poured into a sieve, the remainder remaining on the sieve was flushed back into the beaker with water and dispersed again with the same amount of water, poured into the sieve as described previously, and the operation was repeated twice more. Washing all residues in a beaker with water, flushing the residues on a screen by using a sprinkler connected with a water supply device with a water level difference of 1m until the washing liquid is clear, lightly brushing the residues with a hairbrush if necessary, washing the residues into a glass sand core crucible which is baked at 105+/-2 ℃ in advance and has constant mass, carrying out suction filtration, and placing the glass sand core crucible in a constant-temperature drying oven at 105+/-2 ℃ for drying until the mass is constant.
Note that: the test water is tap water filtered by a test sieve with 0.038mm
1.9.4 results calculation
Fineness is calculated as mass fraction W6, and the value is expressed in%, calculated as formula (6):
wherein:
m 1-the mass of the screen residue in grams (g);
m is the value of the sample mass, and the unit is gram (g).
Taking the arithmetic average value of the parallel measurement results as the measurement result, wherein the absolute difference of the two parallel measurement results is not more than 0.03%.
1.10 determination of particle size distribution
1.10.1 method summary
Like GB/T19077.1-2003 chapter IV.
1.10.2 reagent
Sodium hexametaphosphate solution: 0.2%.
1.10.3 instruments
1.10.3.1 laser granulometry: JL-1177 type
Measuring range: 0.02-2000 um;
precision: 1%.
1.10.3.2 ultrasonic dispersing instrument
1.10.4 analytical procedure
And (3) switching on the power supply of the instrument and preheating the instrument for more than 30 minutes. About 300mL (at about 2/3 of the cell) of 0.2% sodium hexametaphosphate was added to the cell. And opening the computer, running a desktop icon JL-1177 test program on the computer, entering a test program interface, and opening a circulating pump to circulate water. Clicking the instrument zeroing on the menu bar, displaying the desktop with the blank test, clicking the blank test on the menu bar, displaying the desktop with the normal state, the powder adding test, clicking the powder adding preparation on the menu bar, adding a proper amount of powder into the sample pool, and ensuring the relative adding amount concentration to be displayed between 55 and 85. The computer automatically completes the first test, after displaying the data, can continue clicking the test button for 3-5 times, and after the data is stable, the test result is recorded and stored. After the test is finished, the cleaning machine firstly turns off the power supply of the instrument and then turns off the power supply of the computer.
1.11 conductivity
1.11.1 reagents
1.11.1.1 pure water: the conductivity is not more than 4 mu s-cm-1.
1.11.1.2 absolute ethyl alcohol: the conductivity is not more than 4 mu s-cm-1.
1.11.2 instrument
1.11.2.1 centrifuges or high-speed centrifuges.
1.11.2.2 Filter paper: fine, washing with pure water to a conductivity of not more than 5 μs-cm-1.
1.11.2.3 barrel (beaker): about 35mm in diameter, about 125mm in depth, or other suitable electrical conductivity greater than 5 mus-cm-1.
1.11.2.4 thermometer: the minimum index is 0.2 ℃.
1.11.2.5 conductivity meter.
1.11.2.6 electrically conductive electrode: the conductivity cell constant K is about 1.
1.11.3 step
1.11.3.1 sample
Weigh 5g of sample and place in a 250mL beaker. 100mL of pure water, 1mL of absolute ethanol was added, heated under reflux for 10min, cooled and filtered with filter paper, or the solid was separated by centrifuge or high-speed centrifuge, at which time the test tube was washed and dried or rinsed with a small amount of slurry, and the supernatant was filtered through filter paper. In either case, the first 20mL of filtrate was discarded.
1.11.3.2 assay
The filtrate was cooled to about 20 ℃. Both the cylinder (beaker) (5.13.2.3) and the conductance electrode (5.13.2.6) were rinsed first with pure water and then with filtrate. The cylinder (beaker) is filled with filtrate and the conductive electrode is then placed. The conductance electrode is moved up and down to expel air bubbles. The filtrate temperature was adjusted slowly to 23℃and the conductivity electrode was immersed approximately 10mm below the liquid surface, in a position standing in the middle of the cylinder (beaker), and measured at least 5 times with a conductivity meter with an amplifying device at a temperature of (23.+ -. 0.5). Degree.C, the meter was provided with a conductivity cell constant adjusting device, and the read value was conductivity Lt.
The entire operation described above is repeated.
1.11.4 the results show that
The results of the conductivity meter measurements were recorded and the average of the secondary measurements was taken and the results were accurate to 1% of the values obtained.
1.12 determination of sulfide content
1.12.1 method summary
In an acidic solution, the reaction sample of S2-and iodine solution is added with excessive iodine to reduce S2-, and the residual iodine is titrated by using a sodium thiosulfate standard solution, and the content of S2-is calculated according to the titration amount.
1.12.2 reagents and apparatus
1.12.2.1 acetic acid solution: 1+4
1.12.2.2 iodine solution: 0.01mol/L;
10mL of the 0.1mol/L iodine standard solution prepared according to 5.9.1 in HG/T3696.1-2011 was pipetted into a 100mL brown volumetric flask, diluted to scale with water, and shaken well.
1.12.2.3 sodium thiosulfate standard titration solution: c (Na 2S2 O3.apprxeq.0.01 moL/L)
25mL of the 0.1mol/L sodium thiosulfate standard solution prepared according to 5.6 in HG/T3696.1-2011 was pipetted into a 250mL volumetric flask, diluted to scale with water and shaken well.
1.12.2.4 soluble starch solution: 5g/L
1.12.2.5 iodometric flask: 250mL
1.12.2.6 microtiter tubes: the index value was 0.01mL or 0.02mL.
1.12.3 analytical procedure
About 10g of the sample is weighed to the accuracy of 0.01g, placed in a 250mL volumetric flask, 100mL of water is added, a plug is covered, shaking vigorously for 2 minutes, diluting with water until shaking to a scale, filtering, discarding the initial 20mL, re-filtering if the solution is turbid, transferring 100mL of filtrate into a 250mL iodometric flask, transferring 5mL of iodine solution into the solution by a pipette, adding 5mL of acetic acid solution, covering a bottle stopper, sealing the water, shaking, and placing in the dark for 5 minutes. Excess iodine was titrated with a standard titration solution of sodium thiosulfate, and 2mL of starch solution was added near the endpoint, and the titration continued until blue disappeared and no longer appeared within 30 seconds. And simultaneously, blank samples are prepared.
Representation of 1.12.4 analysis results
The content (w 7) of sulfide (S2-) expressed in mass percent is calculated according to formula (7):
wherein: c-concentration of sodium thiosulfate standard titration solution, moL/L
v 0-titration volume for blank, mL
V1-titration volume of sample test, mL
m-mass of sample, g
0.01603A 1mL sodium thiosulfate solution corresponds to the milliequivalents of S.
2. Test results
The purity of the sodium sulfide crystals obtained in examples 1 to 6 and comparative examples 2 to 3 was measured by the above-mentioned method, and the results are shown in Table 1
Table 1 summary of test results for various indexes of barium sulfate
The present invention has been disclosed above in terms of preferred embodiments, but it will be understood by those skilled in the art that these embodiments are merely illustrative of the present invention and should not be construed as limiting the scope of the present invention. It should be noted that all changes and substitutions equivalent to those of the embodiments are intended to be included within the scope of the claims of the present invention. The scope of the invention should, therefore, be determined with reference to the appended claims.
Claims (8)
1. The preparation method of the barium sulfate is characterized by comprising the following steps of:
(1) Respectively carrying out filter pressing on the crude barium sulfide solution and the crude sodium sulfate solution to obtain a barium sulfide solution and a sodium sulfate solution;
(2) Feeding a barium sulfide solution and a sodium sulfate solution into a microcavity reactor for reaction to obtain barium slurry;
(3) The barium slurry automatically flows into a curing tank to carry out curing reaction, so as to obtain product slurry;
(4) Washing and drying a solid phase obtained by solid-liquid separation of the product slurry to obtain powder barium sulfate.
2. The method according to claim 1, wherein in the step (4), the sodium sulfide is obtained by evaporating and flaking a liquid phase obtained by solid-liquid separation of the product slurry.
3. The method according to claim 2, wherein the evaporated condensate in step (4) is used for washing a solid phase obtained by subjecting the product slurry to solid-liquid separation, and the obtained washing water is used for preparing the crude barium sulfide solution and the crude sodium sulfate solution in step (1).
4. The process according to claim 1, wherein in step (1), the concentration of the crude barium sulfide solution is 10% to 15%, the concentration of the crude sodium sulfate solution is 25% to 30%, and the press filtration is performed at 60 ℃ to 70 ℃.
5. According to claimThe process according to claim 1, wherein in the step (2), the barium sulfide solution is fed into the microcavity reactor at a rate of 12m 3 /h～17m 3 The rate of sodium sulfate solution input into the microcavity reactor was 2m 3 /h～7m 3 And/h, the stirring rotating speed of the microcavity reactor is 495 r/min-505 r/min.
6. The method according to claim 1, wherein in the step (3), the aging reaction comprises adding a sodium sulfate solution to the barium slurry to adjust the reaction end point, thereby causing the barium slurry to be slightly over-nitrated.
7. Barium sulfate, characterized in that it is prepared by the preparation method according to any one of claims 1 to 6.
8. The barium sulfate according to claim 7, wherein the particle diameter D50 is 0.30 to 0.80 μm and the whiteness is 99 or more.
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| CN115554958A (en) * | 2022-08-29 | 2023-01-03 | 平利县安得利新材料有限公司 | System and method capable of continuously controlling production of barium sulfate with different particle sizes |
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| CN110155954A (en) * | 2019-04-24 | 2019-08-23 | 贵州红星发展股份有限公司 | A kind of preparation method of high-purity sodium sulfide crystal |
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