CN105502425A - Method for preparing sodium metasilicate nonahydrate by using waste boron mud residue - Google Patents
Method for preparing sodium metasilicate nonahydrate by using waste boron mud residue Download PDFInfo
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- CN105502425A CN105502425A CN201410478025.2A CN201410478025A CN105502425A CN 105502425 A CN105502425 A CN 105502425A CN 201410478025 A CN201410478025 A CN 201410478025A CN 105502425 A CN105502425 A CN 105502425A
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- CN
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- Prior art keywords
- boron mud
- filtrate
- sodium metasilicate
- carrying
- clarification
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- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 title claims abstract description 44
- 229910052796 boron Inorganic materials 0.000 title claims abstract description 44
- 238000000034 method Methods 0.000 title claims abstract description 13
- 239000002699 waste material Substances 0.000 title abstract description 15
- PHIQPXBZDGYJOG-UHFFFAOYSA-N sodium silicate nonahydrate Chemical compound O.O.O.O.O.O.O.O.O.[Na+].[Na+].[O-][Si]([O-])=O PHIQPXBZDGYJOG-UHFFFAOYSA-N 0.000 title abstract 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 38
- 239000000706 filtrate Substances 0.000 claims abstract description 32
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 19
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims abstract description 16
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 15
- 238000006243 chemical reaction Methods 0.000 claims abstract description 14
- 239000013078 crystal Substances 0.000 claims abstract description 14
- 239000012065 filter cake Substances 0.000 claims abstract description 12
- 238000010438 heat treatment Methods 0.000 claims abstract description 12
- 238000003756 stirring Methods 0.000 claims abstract description 12
- 239000000047 product Substances 0.000 claims abstract description 11
- 239000000243 solution Substances 0.000 claims abstract description 9
- 229910000029 sodium carbonate Inorganic materials 0.000 claims abstract description 8
- 239000007864 aqueous solution Substances 0.000 claims abstract description 7
- 238000001816 cooling Methods 0.000 claims abstract description 7
- 238000004821 distillation Methods 0.000 claims abstract description 7
- 238000005260 corrosion Methods 0.000 claims abstract description 6
- TWRXJAOTZQYOKJ-UHFFFAOYSA-L Magnesium chloride Chemical compound [Mg+2].[Cl-].[Cl-] TWRXJAOTZQYOKJ-UHFFFAOYSA-L 0.000 claims description 22
- 238000005352 clarification Methods 0.000 claims description 21
- 235000012239 silicon dioxide Nutrition 0.000 claims description 17
- 229960001866 silicon dioxide Drugs 0.000 claims description 17
- 239000004115 Sodium Silicate Substances 0.000 claims description 15
- 235000019795 sodium metasilicate Nutrition 0.000 claims description 15
- 229910052911 sodium silicate Inorganic materials 0.000 claims description 15
- NASFKTWZWDYFER-UHFFFAOYSA-N sodium;hydrate Chemical compound O.[Na] NASFKTWZWDYFER-UHFFFAOYSA-N 0.000 claims description 14
- 229910001629 magnesium chloride Inorganic materials 0.000 claims description 11
- 229910052710 silicon Inorganic materials 0.000 claims description 9
- 239000010703 silicon Substances 0.000 claims description 9
- 238000002425 crystallisation Methods 0.000 claims description 7
- 239000012535 impurity Substances 0.000 claims description 7
- 239000010802 sludge Substances 0.000 claims description 7
- 230000008025 crystallization Effects 0.000 claims description 6
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 claims description 5
- 238000005842 biochemical reaction Methods 0.000 claims description 5
- 238000007664 blowing Methods 0.000 claims description 5
- 239000001110 calcium chloride Substances 0.000 claims description 5
- 229910001628 calcium chloride Inorganic materials 0.000 claims description 5
- 230000007797 corrosion Effects 0.000 claims description 5
- CNFDGXZLMLFIJV-UHFFFAOYSA-L manganese(II) chloride tetrahydrate Chemical compound O.O.O.O.[Cl-].[Cl-].[Mn+2] CNFDGXZLMLFIJV-UHFFFAOYSA-L 0.000 claims description 5
- 238000000926 separation method Methods 0.000 claims description 5
- 238000001914 filtration Methods 0.000 abstract description 5
- DHRRIBDTHFBPNG-UHFFFAOYSA-L magnesium dichloride hexahydrate Chemical compound O.O.O.O.O.O.[Mg+2].[Cl-].[Cl-] DHRRIBDTHFBPNG-UHFFFAOYSA-L 0.000 abstract 2
- 238000007599 discharging Methods 0.000 abstract 1
- 238000001035 drying Methods 0.000 abstract 1
- 230000000717 retained effect Effects 0.000 abstract 1
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 11
- 239000000395 magnesium oxide Substances 0.000 description 10
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 description 9
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 8
- 235000017550 sodium carbonate Nutrition 0.000 description 6
- 229910021538 borax Inorganic materials 0.000 description 5
- 239000004328 sodium tetraborate Substances 0.000 description 5
- 235000010339 sodium tetraborate Nutrition 0.000 description 5
- 239000000126 substance Substances 0.000 description 5
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 4
- 150000001875 compounds Chemical class 0.000 description 4
- 239000011777 magnesium Substances 0.000 description 4
- 229910052749 magnesium Inorganic materials 0.000 description 4
- ZLNQQNXFFQJAID-UHFFFAOYSA-L magnesium carbonate Chemical compound [Mg+2].[O-]C([O-])=O ZLNQQNXFFQJAID-UHFFFAOYSA-L 0.000 description 3
- 239000011734 sodium Substances 0.000 description 3
- AMWRITDGCCNYAT-UHFFFAOYSA-L hydroxy(oxo)manganese;manganese Chemical compound [Mn].O[Mn]=O.O[Mn]=O AMWRITDGCCNYAT-UHFFFAOYSA-L 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 description 2
- 239000004484 Briquette Substances 0.000 description 1
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- 229910004298 SiO 2 Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 150000001639 boron compounds Chemical class 0.000 description 1
- 229910052810 boron oxide Inorganic materials 0.000 description 1
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 description 1
- 239000000292 calcium oxide Substances 0.000 description 1
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 description 1
- 235000011089 carbon dioxide Nutrition 0.000 description 1
- 239000003245 coal Substances 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- JKWMSGQKBLHBQQ-UHFFFAOYSA-N diboron trioxide Chemical compound O=BOB=O JKWMSGQKBLHBQQ-UHFFFAOYSA-N 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000000284 extract Substances 0.000 description 1
- 239000003337 fertilizer Substances 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 239000001095 magnesium carbonate Substances 0.000 description 1
- 235000014380 magnesium carbonate Nutrition 0.000 description 1
- 229960001708 magnesium carbonate Drugs 0.000 description 1
- 229910000021 magnesium carbonate Inorganic materials 0.000 description 1
- 150000002681 magnesium compounds Chemical class 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- VUZPPFZMUPKLLV-UHFFFAOYSA-N methane;hydrate Chemical compound C.O VUZPPFZMUPKLLV-UHFFFAOYSA-N 0.000 description 1
- 235000010755 mineral Nutrition 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 235000019353 potassium silicate Nutrition 0.000 description 1
- 238000010298 pulverizing process Methods 0.000 description 1
- 239000005060 rubber Substances 0.000 description 1
- HQAITFAUVZBHNB-UHFFFAOYSA-N sodium;pentahydrate Chemical compound O.O.O.O.O.[Na] HQAITFAUVZBHNB-UHFFFAOYSA-N 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000002910 solid waste Substances 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
Landscapes
- Treatment Of Sludge (AREA)
- Silicon Compounds (AREA)
Abstract
The invention relates to a method for preparing sodium metasilicate nonahydrate by using waste boron mud residue. The method comprises: heating boron mud by using steam to achieve a temperature of 59-81 DEG C, maintaining for 1-2 h, and carrying out centrifugal drying through a centrifuge to obtain filter cake boron mud; carrying out a reaction on the filter cake boron mud and hydrochloric acid in an anti-corrosion first reactor according to a pure mass ratio of 1:1.62-2.04, carrying out a chemical reaction under gentle stirring to generate a magnesium chloride hydrate, and filtering the magnesium chloride hydrate to obtain silica filtration residue; and carrying out a reaction on the silica filtration residue and sodium carbonate in a closed second reactor according to a pure mass ratio of 1:1.53-1.95, carrying out heating pressurization and gentle stirring to generate a sodium metasilicate nonahydrate aqueous solution, filtering, conveying the filtrate into a pressure reducing distiller, carrying out distillation concentration, discharging when only nine crystal water are retained in the solution, cooling, and crystallizing to obtain the sodium metasilicate nonahydrate crystal product. According to the present invention, the re-polluted waste material of the boron mud waste material is treated, such that the secondary pollution is avoided, and the economic benefits are created.
Description
Technical field
The present invention relates to the technical field of the inorganic chemical industry disposal of three wastes and comprehensive utilization, particularly relate to a kind of method utilizing useless boron sludge to prepare the inclined silicon of nine water.
Background technology
Boron mud is with szaibelyite (2MgOB
2o
3h
2o) be raw material, by roasting, pulverizing, mix with soda ash, take carbon water law to produce borax (Na
2b
4o
710H
2o), remaining after washing, crystallisation process extract borax solid waste.Produce one ton of borax and can produce 4 tons of boron mud, produce the borax plant of 8000 tons per year for one, can produce boron mud is every year 3.2 ten thousand tons.Because the quantity discharged of boron mud is comparatively large, the multiple comprehensive Utilization Ways of current domestic employing, except production Magnesium Carbonate Light 41-45 and magnesium oxide and plastic and rubber filler, also have produce Peng Mei phosphorus composite fertilizer, to make the coal of honeycomb briquette reinforced and do architectural borax etc.
Magnesium in boron mud is all generally exist with the form of magnesiumcarbonate, sometimes also has difference along with the mineral products difference of szaibelyite.The component of producing Magnesium Carbonate Light 41-45 boron mud is such: magnesium oxide 38%, silicon-dioxide 20%, carbonic acid gas 17%, boron oxide 3%, calcium oxide 3% and manganese oxide 0.11%, other are moisture content.Form solution with boron mud waste material for raw material makes it to become muriate by hydrochloric acid, remove the compound that insoluble impurity obtains the magnesium clarified.Then at the compound of other magnesium of processing, compound of boron etc. is also had.Therefore, be impeccable with regard to the purity of product, quality also reaches a standard.
After the improvement of boron mud and utilization obtain magnesium compound and boron compound, remaining filtration waste residue is only remaining to be difficult to carry out the silicon-dioxide of chemical reaction, its content reaches 80 ~ 90%, now develop silicon goods to be necessary, so through research, successively obtain water glass, zero water sodium metasilicate, metasilicate pentahydrate sodium and non-hydrate sodium metasilicate.
Summary of the invention
Technical problem to be solved by this invention is, the waste material of pollution again of boron mud waste material is processed, comprehensive utilization, outside the compound of output magnesium and boron, also produce silicon product, both avoided secondary pollution, can create very large economic benefit for enterprise again, be the model of the chemical industry comprehensive regulation and utilization.
The technical solution adopted for the present invention to solve the technical problems is: a kind of method utilizing useless boron sludge to prepare the inclined silicon of nine water, comprises the steps:
By boron mud steam heating to 59 ~ 81 degree, maintain 1 ~ 2 hour, then dry with whizzer, realize solid-liquor separation, obtain filtrate and filter cake boron mud, filtrate sends to deep processing separately;
Filter cake boron mud (magnesium oxide meter) and hydrochloric acid are reacted in corrosion resistant first reactor with pure mass ratio 1: 1.62 ~ 2.04, blowing slowly, stirring issues biochemical reaction, reaction generates the hydrate of magnesium chloride, other components generate calcium chloride and a small amount of Manganous chloride tetrahydrate, the hydrate of magnesium chloride is filtered, obtain filtrate and the silicon-dioxide filter residue of clarification, the filtrate of clarification sends to other deep processing;
Silicon-dioxide filter residue and sodium carbonate are reacted in the second airtight reactor with pure mass ratio 1: 1.53 ~ 1.95, under the condition of heating, stirring of pressurizeing and blow slowly, reaction generates the non-hydrate sodium metasilicate aqueous solution, crosses and filters insoluble impurity, obtains the filtrate of clarification;
The filtrate of clarification is sent to underpressure distillation device and carries out inspissation, eject cooling, crystallization when solution inspissation reaches and only remains nine crystal water, obtain non-hydrate sodium metasilicate crystal product.
Its chemical equation is:
MgO+2HCl＝MgCl
2+H
2O
SiO
2+Na
2CO
3+9H
2O＝Na
2SiO
3·9H
2O+CO
2↑
The invention has the beneficial effects as follows: the again pollution waste material of the present invention to boron mud waste material processes, pass through HCl treatment, generate the hydrate of magnesium chloride, filter, obtain silicon-dioxide filter residue, by silicon-dioxide filter residue and sodium carbonate process, generate the non-hydrate sodium metasilicate aqueous solution, remove insoluble impurity, the filtrate of clarification is sent to underpressure distillation device and carries out inspissation, eject cooling, crystallization when solution inspissation reaches and only remains nine crystal water, obtain non-hydrate sodium metasilicate crystal product, therefore, be impeccable with regard to the purity of product, quality also reaches a standard.The again pollution waste material of enterprise to boron mud waste material fully utilizes; obtain non-hydrate sodium metasilicate; turn waste into wealth; improve the ability of enterprise's deep processing; to enterprise development, there is very large pushing effect, while improvement chemical solids waste material, the requirement of environment protection can be met; can also create very large economic benefit to enterprise, be the model of the chemical industry comprehensive regulation and utilization.
Embodiment
Embodiment 1, a kind of method utilizing useless boron sludge to prepare the inclined silicon of nine water described in the present embodiment, comprises the steps:
Get 500 kilograms of boron mud (silicon-dioxide accounts for 20%, and magnesium oxide accounts for 38%) to react, by boron mud steam heating to 59 ~ 81 degree, maintain 1 ~ 2 hour, then dry with whizzer, realize solid-liquor separation, obtain filtrate and filter cake boron mud, filtrate sends to deep processing separately;
Filter cake boron mud (magnesium oxide meter) and hydrochloric acid are reacted in corrosion resistant first reactor with pure mass ratio 1: 1.83, blowing slowly, stirring issues biochemical reaction, reaction generates the hydrate of magnesium chloride, other components generate calcium chloride and a small amount of Manganous chloride tetrahydrate, the hydrate of magnesium chloride is filtered, obtain filtrate and the silicon-dioxide filter residue of clarification, the filtrate of clarification sends to other deep processing;
React in the second airtight reactor by silicon-dioxide filter residue and sodium carbonate with pure mass ratio 1: 1.74, under heating, pressurization and the condition that slowly stirs, reaction generates the non-hydrate sodium metasilicate aqueous solution, crosses and filters insoluble impurity, obtains the filtrate of clarification;
The filtrate of clarification is sent to underpressure distillation device and carries out inspissation, eject cooling, crystallization when solution inspissation reaches and only remains nine crystal water, obtain 466.2 kilograms of non-hydrate sodium metasilicate crystal products.
Embodiment 2, a kind of method utilizing useless boron sludge to prepare the inclined silicon of nine water described in the present embodiment, comprises the steps:
Get 500 kilograms of boron mud (silicon-dioxide accounts for 20%, and magnesium oxide accounts for 38%) to react, by boron mud steam heating to 59 ~ 81 degree, maintain 1 ~ 2 hour, then dry with whizzer, realize solid-liquor separation, obtain filtrate and filter cake boron mud, filtrate sends to deep processing separately;
Filter cake boron mud (magnesium oxide meter) and hydrochloric acid are reacted in corrosion resistant first reactor with pure mass ratio 1: 2.03, blowing slowly, stirring issues biochemical reaction, reaction generates the hydrate of magnesium chloride, other components generate calcium chloride and a small amount of Manganous chloride tetrahydrate, the hydrate of magnesium chloride is filtered, obtain filtrate and the silicon-dioxide filter residue of clarification, the filtrate of clarification sends to other deep processing;
React in the second airtight reactor by silicon-dioxide filter residue and sodium carbonate with pure mass ratio 1: 1.94, under heating, pressurization and the condition that slowly stirs, reaction generates the non-hydrate sodium metasilicate aqueous solution, crosses and filters insoluble impurity, obtains the filtrate of clarification;
The filtrate of clarification is sent to underpressure distillation device and carries out inspissation, eject cooling, crystallization when solution inspissation reaches and only remains nine crystal water, obtain 519.8 kilograms of non-hydrate sodium metasilicate crystal products.
Embodiment 3, a kind of method utilizing useless boron sludge to prepare the inclined silicon of nine water described in the present embodiment, comprises the steps:
Get 500 kilograms of boron mud (silicon-dioxide accounts for 20%, and magnesium oxide accounts for 38%) to react, by boron mud steam heating to 59 ~ 81 degree, maintain 1 ~ 2 hour, then dry with whizzer, realize solid-liquor separation, obtain filtrate and filter cake boron mud, filtrate sends to deep processing separately;
Filter cake boron mud (magnesium oxide meter) and hydrochloric acid are reacted in corrosion resistant first reactor with pure mass ratio 1: 1.63, blowing slowly, stirring issues biochemical reaction, reaction generates the hydrate of magnesium chloride, other components generate calcium chloride and a small amount of Manganous chloride tetrahydrate, the hydrate of magnesium chloride is filtered, obtain filtrate and the silicon-dioxide filter residue of clarification, the filtrate of clarification sends to other deep processing;
React in the second airtight reactor by silicon-dioxide filter residue and sodium carbonate with pure mass ratio 1: 1.54, under heating, pressurization and the condition that slowly stirs, reaction generates the non-hydrate sodium metasilicate aqueous solution, crosses and filters insoluble impurity, obtains the filtrate of clarification;
The filtrate of clarification is sent to underpressure distillation device and carries out inspissation, eject cooling, crystallization when solution inspissation reaches and only remains nine crystal water, obtain 412.6 kilograms of non-hydrate sodium metasilicate crystal products.
The above is only three preferred embodiments of the present invention, is not used for limiting the present invention, and its similar embodiments all, all should be covered by the protection domain of patent of the present invention.
Claims (1)
1. utilize useless boron sludge to prepare a method for the inclined silicon of nine water, it is characterized in that comprising the steps: by boron mud steam heating to 59 ~ 81 degree, maintain 1 ~ 2 hour, then dry with whizzer, realize solid-liquor separation, obtain filtrate and filter cake boron mud, filtrate sends to deep processing separately; Filter cake boron mud and hydrochloric acid are reacted in corrosion resistant first reactor with pure mass ratio 1: 1.62 ~ 2.04, blowing slowly, stirring issues biochemical reaction, reaction generates the hydrate of magnesium chloride, other components generate calcium chloride and a small amount of Manganous chloride tetrahydrate, the hydrate of magnesium chloride is filtered, obtain filtrate and the silicon-dioxide filter residue of clarification, the filtrate of clarification sends to other deep processing; Silicon-dioxide filter residue and sodium carbonate are reacted in the second airtight reactor with pure mass ratio 1: 1.53 ~ 1.95, under the condition of heating, stirring of pressurizeing and blow slowly, reaction generates the non-hydrate sodium metasilicate aqueous solution, crosses and filters insoluble impurity, obtains the filtrate of clarification; The filtrate of clarification is sent to underpressure distillation device and carries out inspissation, eject cooling, crystallization when solution inspissation reaches and only remains nine crystal water, obtain non-hydrate sodium metasilicate crystal product.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410478025.2A CN105502425A (en) | 2014-09-12 | 2014-09-12 | Method for preparing sodium metasilicate nonahydrate by using waste boron mud residue |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410478025.2A CN105502425A (en) | 2014-09-12 | 2014-09-12 | Method for preparing sodium metasilicate nonahydrate by using waste boron mud residue |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN105502425A true CN105502425A (en) | 2016-04-20 |
Family
ID=55710811
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201410478025.2A Pending CN105502425A (en) | 2014-09-12 | 2014-09-12 | Method for preparing sodium metasilicate nonahydrate by using waste boron mud residue |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN105502425A (en) |
-
2014
- 2014-09-12 CN CN201410478025.2A patent/CN105502425A/en active Pending
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Application publication date: 20160420 |