CN110482605A - A kind of method and device preparing sodium dichromate using chromite as one step of raw material - Google Patents
A kind of method and device preparing sodium dichromate using chromite as one step of raw material Download PDFInfo
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- CN110482605A CN110482605A CN201910805430.3A CN201910805430A CN110482605A CN 110482605 A CN110482605 A CN 110482605A CN 201910805430 A CN201910805430 A CN 201910805430A CN 110482605 A CN110482605 A CN 110482605A
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- chromite
- tank
- sodium
- carbon dioxide
- raw material
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- JHWIEAWILPSRMU-UHFFFAOYSA-N 2-methyl-3-pyrimidin-4-ylpropanoic acid Chemical compound OC(=O)C(C)CC1=CC=NC=N1 JHWIEAWILPSRMU-UHFFFAOYSA-N 0.000 title claims abstract description 38
- 238000000034 method Methods 0.000 title claims abstract description 23
- 239000002994 raw material Substances 0.000 title claims abstract description 21
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims abstract description 94
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims abstract description 56
- 239000001569 carbon dioxide Substances 0.000 claims abstract description 48
- 229910002092 carbon dioxide Inorganic materials 0.000 claims abstract description 48
- 238000002156 mixing Methods 0.000 claims abstract description 47
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 claims abstract description 43
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 40
- 239000001301 oxygen Substances 0.000 claims abstract description 40
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 38
- 239000000047 product Substances 0.000 claims abstract description 31
- 229910000029 sodium carbonate Inorganic materials 0.000 claims abstract description 28
- 235000017550 sodium carbonate Nutrition 0.000 claims abstract description 28
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 27
- 239000007789 gas Substances 0.000 claims abstract description 25
- 239000006228 supernatant Substances 0.000 claims abstract description 22
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 22
- 229910001868 water Inorganic materials 0.000 claims abstract description 22
- 235000017557 sodium bicarbonate Nutrition 0.000 claims abstract description 20
- 229910000030 sodium bicarbonate Inorganic materials 0.000 claims abstract description 20
- 239000002699 waste material Substances 0.000 claims abstract description 20
- 239000013078 crystal Substances 0.000 claims abstract description 14
- 239000011344 liquid material Substances 0.000 claims abstract description 12
- 238000001816 cooling Methods 0.000 claims description 28
- 238000003756 stirring Methods 0.000 claims description 28
- 239000007788 liquid Substances 0.000 claims description 23
- 239000000203 mixture Substances 0.000 claims description 14
- 238000004140 cleaning Methods 0.000 claims description 13
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 12
- 239000000498 cooling water Substances 0.000 claims description 11
- 239000000463 material Substances 0.000 claims description 10
- 229910052742 iron Inorganic materials 0.000 claims description 6
- 238000000926 separation method Methods 0.000 claims description 6
- 239000000126 substance Substances 0.000 claims description 5
- 238000007689 inspection Methods 0.000 claims description 4
- UIIMBOGNXHQVGW-DEQYMQKBSA-M Sodium bicarbonate-14C Chemical compound [Na+].O[14C]([O-])=O UIIMBOGNXHQVGW-DEQYMQKBSA-M 0.000 claims description 2
- 238000005086 pumping Methods 0.000 claims 1
- 238000010438 heat treatment Methods 0.000 description 17
- 238000004519 manufacturing process Methods 0.000 description 15
- 239000011651 chromium Substances 0.000 description 8
- 239000011734 sodium Substances 0.000 description 7
- 238000006243 chemical reaction Methods 0.000 description 6
- 230000005611 electricity Effects 0.000 description 6
- 150000003839 salts Chemical class 0.000 description 6
- 238000000354 decomposition reaction Methods 0.000 description 5
- 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 4
- 229910052708 sodium Inorganic materials 0.000 description 4
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 3
- 229910052785 arsenic Inorganic materials 0.000 description 3
- RQNWIZPPADIBDY-UHFFFAOYSA-N arsenic atom Chemical compound [As] RQNWIZPPADIBDY-UHFFFAOYSA-N 0.000 description 3
- 229910052804 chromium Inorganic materials 0.000 description 3
- 229910052500 inorganic mineral Inorganic materials 0.000 description 3
- 230000003834 intracellular effect Effects 0.000 description 3
- 235000010755 mineral Nutrition 0.000 description 3
- 239000011707 mineral Substances 0.000 description 3
- 238000002360 preparation method Methods 0.000 description 3
- 235000008733 Citrus aurantifolia Nutrition 0.000 description 2
- 235000011941 Tilia x europaea Nutrition 0.000 description 2
- 239000006227 byproduct Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 239000004571 lime Substances 0.000 description 2
- 239000010935 stainless steel Substances 0.000 description 2
- 229910001220 stainless steel Inorganic materials 0.000 description 2
- 229910000851 Alloy steel Inorganic materials 0.000 description 1
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 description 1
- 241000196324 Embryophyta Species 0.000 description 1
- 229910000604 Ferrochrome Inorganic materials 0.000 description 1
- 241000237858 Gastropoda Species 0.000 description 1
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- 241001465754 Metazoa Species 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000009529 body temperature measurement Methods 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- KRVSOGSZCMJSLX-UHFFFAOYSA-L chromic acid Substances O[Cr](O)(=O)=O KRVSOGSZCMJSLX-UHFFFAOYSA-L 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- SOCTUWSJJQCPFX-UHFFFAOYSA-N dichromate(2-) Chemical compound [O-][Cr](=O)(=O)O[Cr]([O-])(=O)=O SOCTUWSJJQCPFX-UHFFFAOYSA-N 0.000 description 1
- 229910001882 dioxygen Inorganic materials 0.000 description 1
- 235000021186 dishes Nutrition 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 238000010304 firing Methods 0.000 description 1
- AWJWCTOOIBYHON-UHFFFAOYSA-N furo[3,4-b]pyrazine-5,7-dione Chemical compound C1=CN=C2C(=O)OC(=O)C2=N1 AWJWCTOOIBYHON-UHFFFAOYSA-N 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 230000008774 maternal effect Effects 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000005272 metallurgy Methods 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 238000003541 multi-stage reaction Methods 0.000 description 1
- 238000007747 plating Methods 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 239000011819 refractory material Substances 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 239000002893 slag Substances 0.000 description 1
- 239000002023 wood Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G37/00—Compounds of chromium
- C01G37/14—Chromates; Bichromates
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Processing Of Solid Wastes (AREA)
Abstract
The present invention discloses a kind of method and device that sodium dichromate is prepared using chromite as one step of raw material, obtains mixing liquid material specifically includes the following steps: chromite, soda ash, sodium hydroxide, water are mixed according to mass ratio 1:1 ~ 1.1:0.4 ~ 0.5:5 ratio and are heated to 100 DEG C；Liquid material will be mixed at 3 ~ 3.5Mpa of oxygen pressure, 200 ~ 230 DEG C of temperature, react 2 ~ 3h；After having reacted, oxygen is changed to carbon dioxide gas, air pressure is 1.2 ~ 1.3Mpa, and temperature is 60 ~ 70 DEG C, reacts 2 ~ 3h, obtains product mix；Product mix is separated into supernatant, supernatant obtains the sodium bicarbonate crystal of white at 10 ~ 15 DEG C of temperature, and after sodium bicarbonate is separated, solution is concentrated, is cooled down again, sodium dichromate product is obtained；In the present invention, CO that sodium bicarbonate is decomposed2With sodium carbonate reuse, CO is realized2, soda ash, thermal energy high-efficiency self-circulation utilize, reduce the waste of the energy.
Description
Technical field
The invention belongs to the preparation fields of sodium dichromate, and in particular to a kind of to prepare sodium dichromate by a step of raw material of chromite
Method and device.
Background technique
Chromite is a kind of mineral, and main component is the oxide of iron, magnesium and chromium.Chromite is to develop metallurgy, national defence, change
The indispensable mineral resources of the industry such as work are mainly used for metallurgical industry production stainless steel and various steel alloys, alloy, in glass
Glass, ceramics, refractory material etc. also have extensive use.In addition, be also used to extracting metals chromium, production ferrochrome, stainless steel,
Manufacture bichromate etc..
Chromic salts is widely used in the fields such as plating, coating, wood preservation, wherein maternal product of the sodium dichromate as chromic salts,
70% ~ 85%, for manufacturing other chromic salts products, has very extensive purposes.Chromic acid product salt is usually to be roasted by soda ash
What firing technique obtained, due to environmental problem, roasting technique is faced with huge pressure at present, in sode ash roasting process, furnace charge
It is middle that the lime containing the chromite quality such as almost is added, siliceous in ore and acid gangue mineral are controlled, but the addition of lime can produce
Raw a large amount of high alkalinity chromite processes slag, wherein the Cr VI (mass fraction) containing 1%-2%, will lead to CaCrO4Production
It is raw, CaCrO4It is volatility and airborne, the health of the mankind, animal and plant is caused a significant threat, and this life
Production. art there are serious secondary pollution, the wasting of resources, energy consumption is high, production efficiency is low the problems such as, therefore in order to solve traditional work
Defect existing for skill is badly in need of new technology.
Summary of the invention
The present invention provides a kind of method for preparing sodium dichromate as one step of raw material using chromite, realizes and prepares sodium dichromate process
The high-efficiency self-circulation utilization of element, carbon dioxide, reduces energy waste, and the process for preparing sodium dichromate greatly shortens, and benefit
With the by-product generated in technical process.
A method of sodium dichromate being prepared by one step of raw material of chromite, specifically includes the following steps:
(1) chromite, soda ash, sodium hydroxide, water are mixed and are heated according to mass ratio 1:1 ~ 1.1:0.4 ~ 0.5:5 ratio
Mixing liquid material is obtained to 100 DEG C；
(2) by the mixing liquid material of step (1) at 3 ~ 3.5Mpa of oxygen pressure, 200 ~ 230 DEG C of temperature, 2 ~ 3h is reacted；
(3) after step (2) has been reacted, oxygen is changed to carbon dioxide gas, air pressure is 1.2 ~ 1.3Mpa, and temperature is 60 ~ 70
DEG C, 2 ~ 3h is reacted, product mix is obtained；
(4) step (3) product mix is separated into supernatant, supernatant obtains the sodium bicarbonate of white at 10 ~ 15 DEG C of temperature
Crystal after separating sodium bicarbonate, surplus solution is concentrated at 70 ~ 80 DEG C, is cooled down again, sodium dichromate product is obtained.
The mass percentage content of simple substance Cr is 68% in step (1) chromite, and the purity of soda ash is 99%, sodium hydroxide
Purity be greater than 96%.
Step (4) sodium bicarbonate crystal decomposes at 100 DEG C and obtains sodium carbonate and carbon dioxide, and carbon dioxide returns to step
(3) it uses, sodium carbonate is used back to step (1)；The residue of product mix separation is used to mention iron after being washed with water 1-2 times,
Cleaning solution return step (1)
The present invention also provides the device for preparing sodium dichromate using chromite as one step of raw material, including it is mixing arrangement 1, agitating device, sleeping
Formula reaction kettle 7, waste liquid tank 20, oxygen tank 23, carbon dioxide gas tank 24, decomposition tank 25, knockout drum 26, pump and valve are several, mix
Attach together to set and be equipped with agitating device in 1, mixing arrangement 1 is equipped with 4 feed inlets, a discharge port, discharge port by pump 6 with it is horizontal
The mixed liquor mouth 8 on 7 top of reaction kettle connects, and horizontal reacting kettle 7 is equipped with more than one upper evacuation port 10, oxygen intake
14, carbon dioxide entrance 15, supernatant outlet 16, discharge port 18, more than one lower discharge outlet 21 are equipped at each mouthful
Valve, for being vented and adding water, lower discharge outlet 21 connects for cleaning solution, lower discharge outlet 21 to be discharged with waste liquid tank 20 upper evacuation port 10
It connects, waste liquid tank 20 is connect by pump with the water feed inlet therein of mixing arrangement 1；
Oxygen intake 14 is connect with oxygen tank 23, and carbon dioxide entrance 15 is connect with carbon dioxide gas tank 24,
Supernatant outlet 16 is connect by pump with knockout drum 26, is connected at the top of 26 bottom of knockout drum and decomposition tank 25, is decomposed tank
25, it is equipped with valve between knockout drum 26, decomposes and is connect by pump with carbon dioxide gas tank 24 at the top of tank 25, it is logical to decompose 25 bottom of tank
Pump is crossed to connect with the soda ash feed inlet therein of mixing arrangement 1.
The agitating device includes self-priming paddle 2, motor 3, stirring rod 4, open type worm gear stirring blade 5, stirring rod 4
One end passes through 1 top of mixing arrangement and connect with motor 3, self-priming paddle 2 is equipped in the middle part of stirring rod 4,4 bottom of stirring rod is equipped with
Open type worm gear stirring blade 5.
Adding thermal resistance, thermometer are additionally provided with inside the mixing arrangement 1.
Adding thermal resistance, thermometer 19, pressure gauge 11, liquidometer 12 are additionally provided with inside the horizontal reacting kettle 7.
Cooling device 17 is equipped with outside the horizontal reacting kettle 7, cooling device 17 wraps up 7 lower part of horizontal reacting kettle
Come, be hollow structure inside cooling device 17,17 lower part of cooling device is equipped with cooling water inlet 22, and top is discharged equipped with cooling water
Mouth 13；The identical cooling device with 7 outside of horizontal reacting kettle is equipped with outside the knockout drum 26.
Inspection manhole 9 is additionally provided on the horizontal reacting kettle 7.
Adding thermal resistance, thermometer are equipped in the decomposition tank 25；Adding thermal resistance, thermometer are equipped in knockout drum 26.
Beneficial effects of the present invention:
(1) clean manufacturing: completing sodium dichromate whole process wet method preparation process technology, revolutionizes traditional calcining production mould
Formula, realizes that sodium dichromate manufacturing process flow is simple, and no waste discharge reduces environmental pollution, and reaches plant-scale sodium dichromate
Production model.
(2) realize that the efficient circulation of resource comprehensively utilizes system: obtained sodium bicarbonate decomposes the sodium carbonate generated through transporting
Defeated pipeline is passed through mixing arrangement, and carbon dioxide returns to horizontal reacting kettle, realizes that sodium element, carbon dioxide self-loopa utilize, reduces
Energy waste, the by-product that comprehensive utilization process process generates.
(3) it reduces sodium dichromate manufacturing cost: changing the modes such as the reaction, filtering, evaporation of chromic salts tradition extensive style, introduce
Horizontal reacting kettle, knockout drum decompose tank, and system solves the problems such as equipment attrition is big, chromium yield is low, increases substantially arsenic
The production of sodium.
(4) preparation flow is simple: changing chromic salts tradition stepwise reaction, is during the reaction closed system, operates
Simply, the process for preparing sodium dichromate is greatly shortened, it being capable of the obtained sodium dichromate product of a step.
Detailed description of the invention
Fig. 1 is the structural schematic diagram of 1 device of the embodiment of the present invention；
In figure: 1- mixing arrangement；The self-priming paddle of 2-；3- motor；4- stirring rod；5- open type worm gear stirring blade；6- pump；7-
Horizontal reacting kettle；8- mixed liquor mouth；9- inspection manhole；The upper evacuation port of 10-；11- pressure gauge；12- liquidometer；13- cooling water
Outlet；14- oxygen intake；15- carbon dioxide entrance；16- supernatant outlet；17- cooling device；18- discharge port；19-
Thermometer；20- waste liquid tank；Discharge outlet under 21-；The cooling water inlet 22-；23- oxygen tank；24- carbon dioxide gas tank；25- is decomposed
Tank；26- knockout drum.
Specific embodiment
The invention will be described in further detail with reference to the accompanying drawing, enables those skilled in the art's reference literary
Word is implemented, and what is do not described in detail is that those skilled in the art are clearly commercially available or available by conventional means
Product.
Embodiment 1
A kind of device preparing sodium dichromate using chromite as one step of raw material, as shown in Figure 1, include mixing arrangement 1, agitating device,
Horizontal reacting kettle 7, waste liquid tank 20, oxygen tank 23, carbon dioxide gas tank 24, decomposition tank 25, knockout drum 26, pump and valve are several,
It is additionally provided with adding thermal resistance, thermometer inside mixing arrangement 1, is respectively used to heating and temperature measurement, is equipped with stirring in mixing arrangement 1
Device, agitating device include self-priming paddle 2, motor 3, stirring rod 4, open type worm gear stirring blade 5, and 4 one end of stirring rod is worn
It crosses 1 top of mixing arrangement to connect with motor 3, self-priming paddle 2 is equipped in the middle part of stirring rod 4,4 bottom of stirring rod is equipped with open type snail
Stirring blade 5 is taken turns, self-priming paddle 2 seethes feed liquid upwards, and material is pressed downward by open type worm gear stirring blade 5, so that
Material is mixed and is heated evenly, and reduces heating time, and mixing arrangement 1 is equipped with 4 feed inlets, a discharge port, 4 feed inlets
It is chromite entrance, soda ash entrance, sodium hydroxide entrance, water inlet respectively,
Discharge port 6 is connect by pump with the mixed liquor mouth 8 on 7 top of horizontal reacting kettle, set on horizontal reacting kettle 7 there are two upper row
It eats dishes without rice or wine 18,10, oxygen intake 14, carbon dioxide entrance 15, supernatant outlet 16, discharge port lower discharge outlets 21, each
Be equipped with valve at mouthful, upper evacuation port 10 for being vented and add water, lower discharge outlet 21 for being discharged cleaning solution, lower discharge outlet 21 and
Waste liquid tank 20 connects, and waste liquid tank 20 is connect by pump with one of feed inlet, that is, water inlet of mixing arrangement 1；Oxygen intake 14
It being connect with oxygen tank 23, carbon dioxide entrance 15 is connect with carbon dioxide gas tank 24,
Supernatant outlet 16 is connect by pump with knockout drum 26, is connected at the top of 26 bottom of knockout drum and decomposition tank 25, is decomposed tank
25, it is equipped with valve between knockout drum 26, decomposes and is equipped with adding thermal resistance, thermometer in tank 25, is arranged at and decomposes 25 bottom of tank, point
Solution 25 top of tank is connect by pump with carbon dioxide gas tank 24, is decomposed 25 bottom of tank and is passed through pump and one of them of mixing arrangement 1
Feed inlet, that is, soda ash entrance connects, and is additionally provided with adding thermal resistance, thermometer 19, pressure gauge 11, liquidometer inside horizontal reacting kettle 7
12, in 7 bottom of horizontal reacting kettle, pressure gauge 11, liquidometer 12 are arranged in horizontal reacting kettle 7 for adding thermal resistance, the setting of thermometer 19
Top is equipped with cooling device 17 outside horizontal reacting kettle 7, and cooling device 17 wraps up 7 lower part of horizontal reacting kettle, cooling dress
Setting 17 inside is hollow structure, and 17 lower part of cooling device is equipped with cooling water inlet 22, and top is equipped with cooling water outlet 13；Separation
It is equipped with the identical cooling device with 7 outside of horizontal reacting kettle outside tank 26, is additionally provided with inspection manhole 9 on horizontal reacting kettle 7, is used for
Inside horizontal reacting kettle 7 when something goes wrong, people, which enters, overhauls；Above-mentioned every two component junction is equipped with valve.
The device of the present embodiment is used to prepare sodium dichromate by one step of raw material of chromite, steps are as follows for specific method:
(1) by the mass percentage content containing simple substance Cr be 68% chromite, purity be 99% soda ash, purity be greater than 96%
Sodium hydroxide, water be added in mixing arrangement 1 according to the ratio of mass ratio 1:1:0.4:5, open motor 3 and heating electricity
Resistance, heat while stirring mixing, and thermometer measure temperature stops heating stirring after reaching 100 DEG C, obtains mixing liquid material；
(2) the pressurized pump 6 of the mixing liquid material of step (1) extracted out from the material liquid outlet of mixing arrangement 1 and from mixed liquor mouth 8 into
Enter in horizontal reacting kettle 7, obtains closing on horizontal reacting kettle 7 after the liquid level in horizontal reacting kettle 7 reaches boundary line from liquidometer 12
Each mouth, then open oxygen intake 14 and upper evacuation port 10, oxygen enters in horizontal reacting kettle 7 from oxygen tank 23, is continually fed into
Oxygen ten minutes later, closes each mouth, opens oxygen intake, then leads to oxygen, until pressure gauge 11 shows that pressure to 3Mpa, closes oxygen
Gas entrance 14, the adding thermal resistance opened in horizontal reacting kettle 7 heat materials inside, and 19 displays temperature of thermometer is 200
Stop heating after DEG C, reacts 3h；
(3) after step (2) has been reacted, carbon dioxide entrance 15 and upper evacuation port 10 is opened, carbon dioxide gas 10 is passed through and divides
Clock, evacuation port 10 in closing continue to be passed through carbon dioxide gas to pressure gauge 11 showing that air pressure is 1.2Mpa, while toward cooling dress
It sets in 17 cooling water inlet 22 and injects cold water, cool down, 19 displays temperature of thermometer is 60 DEG C, reacts 3h, is mixed
Product；
(4) by the supernatant of the product mix of step (3) from supernatant outlet 16 with knockout drum 26 is pumped into, in knockout drum
In 26, using 26 outside of knockout drum and identical cooling device outside horizontal reacting kettle 7,26 temperature of knockout drum is down to 10 DEG C of guarantors
Temperature obtains the sodium bicarbonate crystal of white first, when sodium bicarbonate crystal is not further added by, open decompose tank 25 and knockout drum 26 it
Between valve, by sodium bicarbonate crystal from 26 bottom of knockout drum be segregated into decompose tank 25, open knockout drum 26 in heating electricity
Resistance, the remaining solution of knockout drum 26 is heated to 70 DEG C and is concentrated after separation, and thermometer is monitored, and is heated to volume no longer
Liquidometer can be filled after variation, in knockout drum 26 and carries out volume observation, recycle the cooling device cooling outside knockout drum 26 cold
But room temperature is arrived, sodium dichromate product is obtained；
The adding thermal resistance decomposed in tank 25 is opened, is heated to 25 intracellular bicarbonate sodium of tank is decomposed, thermometer display reaches 100 DEG C
Stop heating afterwards, sodium bicarbonate decomposes to obtain sodium carbonate and carbon dioxide, and carbon dioxide is pumped into carbon dioxide gas tank 24, step
Suddenly (2) are spare；After no longer generating carbon dioxide gas, obtained sodium carbonate, which is pumped from soda ash entrance, is pumped into mixing arrangement 1, returns
Return to step (1) use；
From upper evacuation port 10 plus water, after the residue after supernatant is separated to product mix cleans 1 time, open on lower discharge outlet 21
Valve, cleaning solution enter waste liquid tank 20, and the cleaning solution in waste liquid tank 20, which is pumped from water inlet, is pumped into mixing arrangement 1, back to step
Suddenly (1) uses；Residue after cleaning is discharged from discharge port 18 for mentioning iron.
Na in the sodium dichromate product that the present embodiment finally obtains2CrO7·H2The content of O is 98.32%.
Embodiment 2
Using the device of embodiment 1, upper evacuation port and lower evacuation port are one, prepare arsenic by one step of raw material of chromite
Sodium, steps are as follows for specific method:
(1) by the mass percentage content containing simple substance Cr be 68% chromite, purity be 99% soda ash, purity be greater than 96%
Sodium hydroxide, water be added in mixing arrangement 1 according to mass ratio 1:1.05:0.45:5 ratio, open motor 3 and heating electricity
Resistance, heat while stirring mixing, and thermometer measure temperature stops heating stirring after reaching 100 DEG C, obtains mixing liquid material；
(2) the pressurized pump 6 of the mixing liquid material of step (1) extracted out from the material liquid outlet of mixing arrangement 1 and from mixed liquor mouth 8 into
Enter in horizontal reacting kettle 7, from liquidometer 12 obtain the liquid level in horizontal reacting kettle 7 reach reaction boundary line after, close horizontal reacting
After each mouth on kettle 7, then oxygen intake 14 and upper evacuation port 10 are opened, oxygen enters in horizontal reacting kettle 7 from oxygen tank 23, holds
It is continuous to be passed through oxygen ten minutes later, each mouth is closed, oxygen intake is opened, then leads to oxygen, until pressure gauge 11 shows that pressure arrives
3.2Mpa closes oxygen intake 14, and the adding thermal resistance opened in horizontal reacting kettle 7 heats materials inside, thermometer 19
Displays temperature stops heating after being 210 DEG C, reacts 2.5h；
(3) after step (2) has been reacted, carbon dioxide entrance 15 and upper evacuation port 10 is opened, carbon dioxide gas 10 is passed through and divides
Clock, evacuation port 10 in closing continue to be passed through carbon dioxide gas to pressure gauge 11 showing that air pressure is 1.25Mpa, while toward cooling
Cold water is injected in the cooling water inlet 22 of device 17, is cooled down, 19 displays temperature of thermometer is 65 DEG C, reacts 2.5h, obtains
Product mix；
(4) by the supernatant of the product mix of step (3) from supernatant outlet 16 with knockout drum 26 is pumped into, in knockout drum
In 26, using 26 outside of knockout drum and identical cooling device outside horizontal reacting kettle 7,26 temperature of knockout drum is down to 12 DEG C of guarantors
Temperature obtains the sodium bicarbonate crystal of white first, when sodium bicarbonate crystal is not further added by, open decompose tank 25 and knockout drum 26 it
Between valve, by sodium bicarbonate crystal from 26 bottom of knockout drum be segregated into decompose tank 25, open knockout drum 26 in heating electricity
Resistance, the remaining solution of knockout drum 26 is heated to 75 DEG C and is concentrated after separation, and thermometer is monitored, and is heated to volume no longer
Liquidometer can be filled after variation, in knockout drum 26 and carries out volume observation, recycle the cooling device cooling outside knockout drum 26 cold
But room temperature is arrived, sodium dichromate product is obtained；
The adding thermal resistance decomposed in tank 25 is opened, is heated to 25 intracellular bicarbonate sodium of tank is decomposed, thermometer display reaches 100 DEG C
Stop heating afterwards, sodium bicarbonate decomposes to obtain sodium carbonate and carbon dioxide, and carbon dioxide is pumped into carbon dioxide gas tank 24, step
Suddenly (2) are spare；After no longer generating carbon dioxide gas, obtained sodium carbonate, which is pumped from soda ash entrance, is pumped into mixing arrangement 1, returns
Return to step (1) use；
From upper evacuation port 10 plus water, after the residue after supernatant is separated to product mix cleans 1 time, open on lower discharge outlet 21
Valve, cleaning solution enter waste liquid tank 20, and the cleaning solution in waste liquid tank 20, which is pumped from water inlet, is pumped into mixing arrangement 1, back to step
Suddenly (1) uses；Residue after cleaning is discharged from discharge port 18 for mentioning iron.
Na in the sodium dichromate product that the present embodiment finally obtains2CrO7·H2The content of O is 96.22%.
Embodiment 3
Using the device of embodiment 1, upper evacuation port and lower evacuation port are two, prepare arsenic by one step of raw material of chromite
Sodium, steps are as follows for specific method:
(1) by the mass percentage content containing simple substance Cr be 68% chromite, purity be 99% soda ash, purity be greater than 96%
Sodium hydroxide, water be added in mixing arrangement 1 according to mass ratio 1:1.1:0.5:5 ratio, open motor 3 and heating electricity
Resistance, heat while stirring mixing, and thermometer measure temperature stops heating stirring after reaching 100 DEG C, obtains mixing liquid material；
(2) the pressurized pump 6 of the mixing liquid material of step (1) extracted out from the material liquid outlet of mixing arrangement 1 and from mixed liquor mouth 8 into
Enter in horizontal reacting kettle 7, from liquidometer 12 obtain the liquid level in horizontal reacting kettle 7 reach reaction boundary line after, close horizontal reacting
After each mouth on kettle 7, then oxygen intake 14 and upper evacuation port 10 are opened, oxygen enters in horizontal reacting kettle 7 from oxygen tank 23, holds
It is continuous to be passed through oxygen ten minutes later, each mouth is closed, oxygen intake is opened, then leads to oxygen, until pressure gauge 11 shows that pressure arrives
3.5Mpa closes oxygen intake 14, and the adding thermal resistance opened in horizontal reacting kettle 7 heats materials inside, thermometer 19
Displays temperature stops heating after being 230 DEG C, reacts 2h；
(3) after step (2) has been reacted, carbon dioxide entrance 15 and upper evacuation port 10 is opened, carbon dioxide gas 10 is passed through and divides
Clock, evacuation port 10 in closing continue to be passed through carbon dioxide gas to pressure gauge 11 showing that air pressure is 1.3Mpa, while toward cooling dress
It sets in 17 cooling water inlet 22 and injects cold water, cool down, 19 displays temperature of thermometer is 60 DEG C, reacts 2h, is mixed
Product；
(4) by the supernatant of the product mix of step (3) from supernatant outlet 16 with knockout drum 26 is pumped into, in knockout drum
In 26, using 26 outside of knockout drum and identical cooling device outside horizontal reacting kettle 7,26 temperature of knockout drum is down to 15 DEG C of guarantors
Temperature obtains the sodium bicarbonate crystal of white first, when sodium bicarbonate crystal is not further added by, open decompose tank 25 and knockout drum 26 it
Between valve, by sodium bicarbonate crystal from 26 bottom of knockout drum be segregated into decompose tank 25, open knockout drum 26 in heating electricity
Resistance, the remaining solution of knockout drum 26 is heated to 80 DEG C and is concentrated after separation, and thermometer is monitored, and is heated to volume no longer
Liquidometer can be filled after variation, in knockout drum 26 and carries out volume observation, recycle the cooling device cooling outside knockout drum 26 cold
But room temperature is arrived, sodium dichromate product is obtained；
The adding thermal resistance decomposed in tank 25 is opened, is heated to 25 intracellular bicarbonate sodium of tank is decomposed, thermometer display reaches 100 DEG C
Stop heating afterwards, sodium bicarbonate decomposes to obtain sodium carbonate and carbon dioxide, and carbon dioxide is pumped into carbon dioxide gas tank 24, step
Suddenly (2) are spare；After no longer generating carbon dioxide gas, obtained sodium carbonate, which is pumped from soda ash entrance, is pumped into mixing arrangement 1, returns
Return to step (1) use；
From upper evacuation port 10 plus water, after the residue after supernatant is separated to product mix cleans 1 time, open on lower discharge outlet 21
Valve, cleaning solution enter waste liquid tank 20, and the cleaning solution in waste liquid tank 20, which is pumped from water inlet, is pumped into mixing arrangement 1, back to step
Suddenly (1) uses；Residue after cleaning is discharged from discharge port 18 for mentioning iron.
Na in the sodium dichromate product that the present embodiment finally obtains2CrO7·H2The content of O is 97.22%.
Claims (10)
1. a kind of method for preparing sodium dichromate as one step of raw material using chromite, which is characterized in that specifically includes the following steps:
(1) chromite, soda ash, sodium hydroxide, water are mixed and are added according to mass ratio 1:1 ~ 1.1:0.4 ~ 0.5:5 ratio
Heat obtains mixing liquid material to 100 DEG C；
(2) by the mixing liquid material of step (1) at 3 ~ 3.5Mpa of oxygen pressure, 200 ~ 230 DEG C of temperature, 2 ~ 3h is reacted；
(3) after step (2) has been reacted, oxygen is changed to carbon dioxide gas, air pressure is 1.2 ~ 1.3Mpa, and temperature is 60 ~ 70
DEG C, 2 ~ 3h is reacted, product mix is obtained；
(4) step (3) product mix is separated into supernatant, supernatant obtains the sodium bicarbonate of white at 10 ~ 15 DEG C of temperature
After separating sodium bicarbonate, solution is concentrated, is cooled down again, sodium dichromate product is obtained for crystal.
2. the method for preparing sodium dichromate as one step of raw material using chromite according to claim 1, which is characterized in that step (1)
The mass percentage content of simple substance Cr is 68% in chromite, and the purity of soda ash is 99%, and the purity of sodium hydroxide is greater than 96%.
3. the method for preparing sodium dichromate as one step of raw material using chromite according to claim 1, which is characterized in that step (4)
Sodium bicarbonate crystal decomposes at 100 DEG C and obtains sodium carbonate and carbon dioxide, and carbon dioxide is used back to step (3), sodium carbonate
It is used back to step (1)；The residue of product mix separation is used to propose iron, cleaning solution return step after being washed with water 1-2 times
(1).
4. the device of sodium dichromate is prepared described in claim 1 using chromite as one step of raw material, which is characterized in that including mixing arrangement
(1), agitating device, horizontal reacting kettle (7), waste liquid tank (20), oxygen tank (23), carbon dioxide gas tank (24), decompose tank (25),
Knockout drum (26), pump are several, and agitating device is equipped in mixing arrangement (1), and mixing arrangement (1) goes out equipped with 4 feed inlets, one
Material mouth, discharge port are connect by pumping (6) with the mixed liquor mouth (8) on horizontal reacting kettle (7) top, on horizontal reacting kettle (7) also
Equipped with more than one upper evacuation port (10), oxygen intake (14), carbon dioxide entrance (15), supernatant outlet (16), go out
Material mouth (18), more than one lower discharge outlet (21) are equipped with valve at each mouthful, and lower discharge outlet (21) and waste liquid tank (20) are even
It connects, waste liquid tank (20) is connect by pump with one of feed inlet of mixing arrangement (1)；
Oxygen intake (14) is connect with oxygen tank (23), and carbon dioxide entrance (15) is connect with carbon dioxide gas tank (24),
Supernatant outlet (16) is connect by pump with knockout drum (26), and knockout drum (26) bottom connects with tank (25) top is decomposed
It connects, decomposes and be equipped with valve between tank (25) and knockout drum (26), decompose tank (25) side and pass through pump and carbon dioxide gas tank (24)
Connection is decomposed tank (25) bottom and is connect by pump with one of feed inlet of mixing arrangement (1).
5. the device of sodium dichromate is prepared using chromite as one step of raw material according to claim 4, which is characterized in that agitating device
Including self-priming paddle (2), motor (3), stirring rod (4), open type worm gear stirring blade (5), stirring rod (4) one end passes through mixed
It attaches together to set and be connect at the top of (1) with motor (3), be equipped with self-priming paddle (2) in the middle part of stirring rod (4), stirring rod (4) bottom is equipped with
Open type worm gear stirring blade (5).
6. the device of sodium dichromate is prepared using chromite as one step of raw material according to claim 4, which is characterized in that mixing arrangement
(1) internal to be additionally provided with adding thermal resistance, thermometer.
7. the device of sodium dichromate is prepared using chromite as one step of raw material according to claim 4, which is characterized in that horizontal reacting
Adding thermal resistance, thermometer (19), pressure gauge (11), liquidometer (12) are additionally provided with inside kettle (7).
8. the device of sodium dichromate is prepared using chromite as one step of raw material according to claim 4, which is characterized in that horizontal reacting
Cooling device (17) are equipped with outside kettle (7), cooling device (17) wraps up horizontal reacting kettle (7) lower part, cooling device
(17) internal is hollow structure, and cooling device (17) lower part is equipped with cooling water inlet (22), and top is equipped with cooling water outlet
(13)；It is equipped with outside knockout drum (26) and the external identical cooling device of horizontal reacting kettle (7).
9. the device of sodium dichromate is prepared using chromite as one step of raw material according to claim 4, which is characterized in that horizontal reacting
Inspection manhole (9) are additionally provided on kettle (7).
10. the device of sodium dichromate is prepared using chromite as one step of raw material according to claim 4, which is characterized in that decompose tank
(25) and in knockout drum (26) adding thermal resistance, thermometer are equipped with.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102649584A (en) * | 2011-08-22 | 2012-08-29 | 四川省安县银河建化（集团）有限公司 | Preparation method of sodium bichromate |
| CN102897838A (en) * | 2012-11-19 | 2013-01-30 | 四川省安县银河建化（集团）有限公司 | One-step preparation method of sodium bichromate |
| CN103193271A (en) * | 2013-04-02 | 2013-07-10 | 四川省银河化学股份有限公司 | Method for producing high-quality sodium bichromate |
| CN105129852A (en) * | 2015-09-15 | 2015-12-09 | 四川省银河化学股份有限公司 | Efficient self-recycling system for continuously preparing sodium bichromate by wet method |
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2019
- 2019-08-29 CN CN201910805430.3A patent/CN110482605B/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102649584A (en) * | 2011-08-22 | 2012-08-29 | 四川省安县银河建化（集团）有限公司 | Preparation method of sodium bichromate |
| CN102897838A (en) * | 2012-11-19 | 2013-01-30 | 四川省安县银河建化（集团）有限公司 | One-step preparation method of sodium bichromate |
| CN103193271A (en) * | 2013-04-02 | 2013-07-10 | 四川省银河化学股份有限公司 | Method for producing high-quality sodium bichromate |
| CN105129852A (en) * | 2015-09-15 | 2015-12-09 | 四川省银河化学股份有限公司 | Efficient self-recycling system for continuously preparing sodium bichromate by wet method |
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