CN1052097A - Liquid phase circulation replacement process for preparing alkali from mirabilite - Google Patents
Liquid phase circulation replacement process for preparing alkali from mirabilite Download PDFInfo
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- CN1052097A CN1052097A CN 89108806 CN89108806A CN1052097A CN 1052097 A CN1052097 A CN 1052097A CN 89108806 CN89108806 CN 89108806 CN 89108806 A CN89108806 A CN 89108806A CN 1052097 A CN1052097 A CN 1052097A
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- China
- Prior art keywords
- liquid phase
- alkali
- saltcake
- mirabilite
- phenol
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- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 title claims abstract description 30
- 239000007791 liquid phase Substances 0.000 title claims abstract description 9
- 239000003513 alkali Substances 0.000 title abstract description 24
- 238000004519 manufacturing process Methods 0.000 title abstract description 11
- 239000010446 mirabilite Substances 0.000 title abstract description 5
- 238000000034 method Methods 0.000 claims abstract description 23
- 239000002994 raw material Substances 0.000 claims abstract description 7
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 claims description 25
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 20
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 16
- 235000017550 sodium carbonate Nutrition 0.000 claims description 8
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 8
- 235000011121 sodium hydroxide Nutrition 0.000 claims description 7
- 125000004122 cyclic group Chemical group 0.000 claims description 6
- 239000007864 aqueous solution Substances 0.000 claims description 5
- 239000007785 strong electrolyte Substances 0.000 claims description 2
- 239000003245 coal Substances 0.000 abstract description 8
- 238000001354 calcination Methods 0.000 abstract description 3
- 238000006467 substitution reaction Methods 0.000 abstract description 3
- 239000002699 waste material Substances 0.000 abstract description 3
- 238000003837 high-temperature calcination Methods 0.000 abstract description 2
- 238000006243 chemical reaction Methods 0.000 description 22
- 239000003960 organic solvent Substances 0.000 description 13
- 239000000243 solution Substances 0.000 description 12
- 239000011734 sodium Substances 0.000 description 10
- 238000005516 engineering process Methods 0.000 description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 8
- 239000000126 substance Substances 0.000 description 7
- 239000007789 gas Substances 0.000 description 6
- 238000000605 extraction Methods 0.000 description 5
- 239000012071 phase Substances 0.000 description 5
- NESLWCLHZZISNB-UHFFFAOYSA-M sodium phenolate Chemical compound [Na+].[O-]C1=CC=CC=C1 NESLWCLHZZISNB-UHFFFAOYSA-M 0.000 description 5
- 235000008733 Citrus aurantifolia Nutrition 0.000 description 4
- 235000011941 Tilia x europaea Nutrition 0.000 description 4
- 239000011575 calcium Substances 0.000 description 4
- OSGAYBCDTDRGGQ-UHFFFAOYSA-L calcium sulfate Chemical compound [Ca+2].[O-]S([O-])(=O)=O OSGAYBCDTDRGGQ-UHFFFAOYSA-L 0.000 description 4
- 238000005194 fractionation Methods 0.000 description 4
- 239000004571 lime Substances 0.000 description 4
- 239000007788 liquid Substances 0.000 description 4
- 238000002156 mixing Methods 0.000 description 4
- 239000000047 product Substances 0.000 description 4
- 229910052938 sodium sulfate Inorganic materials 0.000 description 4
- 235000011152 sodium sulphate Nutrition 0.000 description 4
- RWSOTUBLDIXVET-UHFFFAOYSA-N Dihydrogen sulfide Chemical compound S RWSOTUBLDIXVET-UHFFFAOYSA-N 0.000 description 3
- 235000019738 Limestone Nutrition 0.000 description 3
- 239000000498 cooling water Substances 0.000 description 3
- 238000011161 development Methods 0.000 description 3
- 238000007599 discharging Methods 0.000 description 3
- 238000005265 energy consumption Methods 0.000 description 3
- 229910000037 hydrogen sulfide Inorganic materials 0.000 description 3
- 239000006028 limestone Substances 0.000 description 3
- 238000001556 precipitation Methods 0.000 description 3
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- 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 2
- 238000009993 causticizing Methods 0.000 description 2
- 239000012141 concentrate Substances 0.000 description 2
- 230000007797 corrosion Effects 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- 238000001704 evaporation Methods 0.000 description 2
- 230000008020 evaporation Effects 0.000 description 2
- 239000000284 extract Substances 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- 239000011259 mixed solution Substances 0.000 description 2
- 238000011084 recovery Methods 0.000 description 2
- 239000011819 refractory material Substances 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 229910052708 sodium Inorganic materials 0.000 description 2
- GRVFOGOEDUUMBP-UHFFFAOYSA-N sodium sulfide (anhydrous) Chemical compound [Na+].[Na+].[S-2] GRVFOGOEDUUMBP-UHFFFAOYSA-N 0.000 description 2
- 239000007790 solid phase Substances 0.000 description 2
- 238000000638 solvent extraction Methods 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- UIIMBOGNXHQVGW-DEQYMQKBSA-M Sodium bicarbonate-14C Chemical compound [Na+].O[14C]([O-])=O UIIMBOGNXHQVGW-DEQYMQKBSA-M 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 description 1
- 239000000920 calcium hydroxide Substances 0.000 description 1
- 229910001861 calcium hydroxide Inorganic materials 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 239000003518 caustics Substances 0.000 description 1
- 238000003889 chemical engineering Methods 0.000 description 1
- 239000002817 coal dust Substances 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 235000009508 confectionery Nutrition 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000001351 cycling effect Effects 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000006073 displacement reaction Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000000706 filtrate Substances 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- -1 hydrogen sodium oxide Chemical class 0.000 description 1
- 238000009434 installation Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 238000002386 leaching Methods 0.000 description 1
- 235000012204 lemonade/lime carbonate Nutrition 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000010309 melting process Methods 0.000 description 1
- 238000005649 metathesis reaction Methods 0.000 description 1
- 239000003345 natural gas Substances 0.000 description 1
- 150000002989 phenols Chemical class 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000011946 reduction process Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 239000013049 sediment Substances 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 229910001948 sodium oxide Inorganic materials 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000003746 solid phase reaction Methods 0.000 description 1
- 238000010671 solid-state reaction Methods 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 238000000967 suction filtration Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 238000003828 vacuum filtration Methods 0.000 description 1
- 239000002912 waste gas Substances 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The new process for preparing alkali from mirabilite-liquid phase circulation substitution method is a new process for preparing alkali by using mirabilite as raw material and using a carrier to make circulation substitution in liquid phase. The invention does not need coal reduction calcination, so huge high-temperature calcination equipment and the like are not needed. Therefore, the method comprises the following steps: energy is saved; secondly, the utilization rate of raw materials is high; investment is saved, and factory building is fast; fourthly, the production process has no three wastes.
Description
The present invention is the novel process that belongs to alkali making technology.
Utilize natural resource saltcake (Na
2SO
4) system alkali is one of important channel during present home and abroad system alkali is produced, the leblanc process of existing more than 200 year history is that coal dust reduction of mirabilite method is still the main production in the present domestic saltcake system alkali industry.Because this method needs to reduce calcination aborning, thereby mainly there is following problem in it:
(1) energy consumption is big, and alkali per ton needs coal (not comprising liquid caustic soda concentrate drying coal) more than 2 tons;
(2) quality product is not good, and prepared using is insufficient, and its main melting process carries out in solid phase, and needs high temperature, and equipment capacity is little, and raw material reaction is incomplete, and sodium utilization is between 60%～80%;
(3) equipment corrosion is serious, workman's labor condition is abominable, since major equipment such as reverberatory furnace or rotary kiln operation at high temperature all the time, the just often replacings such as refractory materials that had a strong impact on by caustic corrosion, and only alkali per ton of the refractory materials of Xiao Haoing just needs about about 50Kg;
(4) pollute greatlyyer, operations such as leaching aborning, filtration just make have an appointment sediment about 1 ton of alkali per ton, almost all have the dust of contaminate environment or gas to discharge in the per pass operation, during carbonating, also have a large amount of hydrogen sulfide dischargings simultaneously.
Since above cause influence be the development of the saltcake basic industry of main production with this method.Thereby the active development utilization to aspects such as the novel process of saltcake system alkali, new technology, new installation, new purposes comes at recent two decades, and particularly in recent years, home and abroad R﹠D institution, universities and colleges, industrial enterprise make great efforts unexpectedly mutually, and do a lot of work.Introduce according to document (1), (2), (3), (4):
(1) national anhydrous sodium sulphate, Sodium Sulphide report of survey
Ruleization office of the Ministry of Chemical Industry, salt affair general bureau of China National Light Industrial Products Department, national anhydrous sodium sulphate, Sodium Sulphide industry information cooperative groups in February, 88
(2) chemical industry Development History
Beijing Chemical Engineering College's chemical industry history is write group
Scientific and technical literature press in March, 85
(3) chemical technology first volume Jiang family fine horse
Higher education press in March, 60
(4) make alkali abroad No. 1, No. 2, No. 3
Design and research institute of Dalian Chemical Industry Co technical information department
In February, 64
Present domestic 40 obtained multinomial scientific payoffss, wherein most to concentrate on the production of natural resource saltcake be on the process for processing technology and equipment of anhydrous sodium sulphate, and few to saltcake alkali-making process aspect.Big quantity research and test have been carried out to the technology (promptly with semi-water gas or Sweet natural gas reduction of mirabilite system alkali) that adopts gas phase reduction process to carry out saltcake system alkali in the home and abroad, but because this technology still needs to carry out under comparatively high temps and need the long reflection time, therefore energy consumption is big, technology is complicated, a large amount of hydrogen sulfide dischargings are arranged simultaneously, so also do not drop into suitability for industrialized production at present.
The object of the present invention is to provide a kind of novel process that adopts liquid phase system alkali, in order to overcoming the deficiency in two kinds of alkali-making process of above-mentioned solid phase and gas phase, to reach the energy consumption of saving in the existing saltcake alkali producing process, to improve raw material availability, reduce cost and reduce purpose such as environmental pollution.
Technical scheme of the present invention is: utilize saltcake (Na in the airtight recycle system
2SO
4) be strong electrolyte, ionization is Na in the aqueous solution
+And SO
2-
4Performance, adopting phenol is that replacement vector carries out cyclic permutation, after carbonating, can obtain soda ash (Na
2CO
3) or the saltcake novel process for making alkaline of caustic soda (NaOH).
Technical ability of the present invention is characterized as:
(1) at saltcake (Na
2SO
4) the aqueous solution in add Ca(OH)
2, just having four kinds of ions in the solution like this is Na
+, SO
- 4, Ca
2+, CH
-, minor N aOH and CaSO are also arranged simultaneously
4Precipitation produces.This process principal reaction formula is:
But, because (OH
-) influence of common-ion effcet, this is reflected at promptly reaches balance after producing minor N aOH, and Ca(OH)
2No longer dissolving, reaction can not continue.But when destroying this (OH
-) after the common-ion effcet, just this reaction might be gone on to the right.
(2) utilize the slightly acidic of the phenolic hydroxyl group of phenol, it can only molten dry hydrogen sodium oxide, and is insoluble to the characteristic of yellow soda ash and sodium bicarbonate, adds phenol in the mixing solutions of saltcake and calcium hydroxide, make minor N aOH reaction in phenol and the mixing solutions, form sodium phenylate and water.This process principal reaction formula is:
②
Reaction formula formation has 2. destroyed (the OH of reaction formula in 1.
-) common-ion effcet, thereby make the Ca(OH of reaction formula in 1.)
2Can continue dissolving and form CaSO simultaneously
4Precipitation, thereby 1. reaction formula can be gone on to the right.The combined reaction formula 1., 2., its chemical equation is:
After sodium phenylate forms, with its process carbonation reaction, then can change Na into again
2CO
3With NaHCO
3, phenol will be separated out again this moment.Its main chemical formula is:
(3) alkali (Na after carbonating
2CO
3, NaHCO
3) and the mixing solutions of phenol, can utilize phenol to be dissolved in organic solvent and alkali is insoluble to the characteristic of organic solvent, the Pyrogentisinic Acid extracts recovery by organic solvent.Organic solvent after the extraction can carry out fractionation according to the different separately boiling point of phenol and organic solvent, and organic solvent is separated with phenol.Phenol after separating and organic solvent can be participated in again with the production of the displacement extraction process of next cycle and use.
The present invention compares with existing saltcake alkali-making process has following characteristics:
(1) save energy.The present invention does not adopt with coal and reduces the incinerating operational path, but adopt with phenol is the operational path that carrier carries out cyclic permutation, compare alkali per ton with former technology and can save coal more than 2 tons (refer to coal combustion and reduction use coal, do not comprise evaporation, the concentrated coal of using).
(2) raw material availability height.The present invention adopts solid state reaction, reacts completely but adopt liquid phase reaction to make, and sodium utilization can reach about 95%, improves about 15% than leblanc process, and phenol wherein is that basic no consumption, lime that is consumed and CO are used in cyclic permutation
2Gas all can be produced through the limestone kiln calcining by natural crystal (Wingdale).
(3) low equipment investment, it is fast to found the factory.The present invention ties up under the normal temperature and carries out, and has then saved huge support equipments such as high-temperature calcination, has also reduced maintenance cost at ordinary times.
(4) not having " three wastes " in the production process pollutes.1. do not have waste water: two water systems are arranged among the present invention, and promptly water of productive use (liquid phase reaction water) all carries out respectively in system separately with cooling water (cooling water during carbonating).Water of productive use ties up in the closed system and carries out, and is evaporation, concentrated at last.All return in the feed proportioning no discharging approach in the use again and tackle the bath water that is carried out in the product calcium sulfate; Cooling water can utilize big cooling pool to recycle.2. do not have waste residue: the solid by product calcium sulfate among the present invention can be made material of construction and use; Lime carbonate can be sent into the limestone kiln again and calcine.3. do not have waste gas: no hydrogen sulfide produces in carbonation.
Accompanying drawing: saltcake system alkali cyclic permutation method process flow sheet.
The present invention is comprised of following three closed-cycle systems:
(1) phenol is in raw material reaction, because the phenolic hydroxyl group reaction forms the mixed solution of sodium phenate and alkali. This Phenol in Aqueous Solution is after being reclaimed by organic solvent extraction, and the circular response that the phenol behind the fractionation organic solvent participates in next cycle again uses.
(2) organic solvent separates with phenol through fractionation by after phenol is reclaimed in extraction from the mixed liquor of phenol and alkali, and the cycling extraction that the organic solvent after the separation participates in again next cycle uses.
(3) utilize limekiln calcined limestone (CaCO3) carbon dioxide that produces carries out carbonation reaction, and participates in simultaneously following reaction and circulation: 1. to the decomposition reaction of saltcake; 2. the causticizing reaction of soda ash (send into the limekiln and again calcine use by the lime deposit after the causticization.
One embodiment of the present of invention:
(1) decomposes replacement(metathesis)reaction: in 1000ml water, add 99% sodium sulfate 198.8 grams (1.4 moles).The dissolving back adds 80% lime 120 grams (excessive), by abundant stirring and progressively add 99% phenol, 263.2 grams (2.8 moles), restir makes abundant reaction after 30 minutes, with solution with the vacuum pump suction filtration and wash three times, collect filtrate 1250ml altogether, this liquid is sodium phenylate solution.
(2) carbonating: sodium phenylate solution is fed content greater than 90% CO
2Gas (steel cylinder dress), this moment, solution began muddiness gradually, and had the yellow soda ash precipitation to produce.Ventilate after a few hours, solution is the mixing solutions of phenol and soda ash, and potential of hydrogen is PH10.
(3) extraction: with organic solvent 2000ml(solution ratio is 1.6) and the mixed solution of phenol and soda ash carry out multi-stage solvent extraction, and isolate light phase and heavy phase with separating funnel, wherein the heavy phase aqueous solution is soda ash liquid.
(4) causticization: this alkali lye is heated, and slowly add with 100 gram lime (excessive), constantly stir, just it carries out causticizing reaction, can get 9% NaOH solution 1150ml behind the vacuum filtration.
(5) phenol recovery: in oil bath organic extract liquid is carried out fractionation with flask, the collection overhead product is an organic solvent, and residuum is a phenol in the bottle.
Claims (1)
- A kind of is the liquid phase cyclic permutation novel process for making alkaline of raw material with the saltcake.Its technical scheme is for to utilize saltcake (Na in the airtight liquid phase recycle system 2SO 4) be strong electrolyte, ionization is Na+ and SO in the aqueous solution 4 2-Performance, adopting phenol is that replacement vector carries out cyclic permutation, after carbonating, can obtain soda ash (Na 2CO 3) or the saltcake novel process for making alkaline of caustic soda (NaOH).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 89108806 CN1052097A (en) | 1989-11-22 | 1989-11-22 | Liquid phase circulation replacement process for preparing alkali from mirabilite |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 89108806 CN1052097A (en) | 1989-11-22 | 1989-11-22 | Liquid phase circulation replacement process for preparing alkali from mirabilite |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN1052097A true CN1052097A (en) | 1991-06-12 |
Family
ID=4857735
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 89108806 Pending CN1052097A (en) | 1989-11-22 | 1989-11-22 | Liquid phase circulation replacement process for preparing alkali from mirabilite |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1052097A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107986299A (en) * | 2017-09-22 | 2018-05-04 | 新疆昌吉职业技术学院 | The method that saltcake liquid phase round-robin method prepares soda ash and caustic soda |
-
1989
- 1989-11-22 CN CN 89108806 patent/CN1052097A/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107986299A (en) * | 2017-09-22 | 2018-05-04 | 新疆昌吉职业技术学院 | The method that saltcake liquid phase round-robin method prepares soda ash and caustic soda |
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