CN102267689A - Production method of sodium sulfide with iron content of less than 30 ppm - Google Patents
Production method of sodium sulfide with iron content of less than 30 ppm Download PDFInfo
- Publication number
- CN102267689A CN102267689A CN 201110190518 CN201110190518A CN102267689A CN 102267689 A CN102267689 A CN 102267689A CN 201110190518 CN201110190518 CN 201110190518 CN 201110190518 A CN201110190518 A CN 201110190518A CN 102267689 A CN102267689 A CN 102267689A
- Authority
- CN
- China
- Prior art keywords
- sodium sulfide
- clear liquid
- iron
- sodium
- sodium sulphite
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Landscapes
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
The invention discloses a production method of sodium sulfide with an iron content of less than 30 ppm so as to solve the present domestic problems of long process flow and environment pollution caused by producing low-iron sodium sulfide by removing iron from zinc salts or barium sulfide. The invention comprises the following steps: mixing a cationic polyacrylamide aqueous solution, which has a mass percent concentration of 0.1%-0.2% and is used as a flocculant, and a sodium sulfide clear liquid with a volume ratio of 1:100-300; stirring for 30-90 minutes under a condition with an insulated temperature of 50 DEG C-60 DEG C; filtering by a plate and frame filter to remove ferrous sulfide daub so as to obtain a low-iron sodium sulfide clear liquid, evaporating the liquid to obtain a sodium sulfide content of 600 g/L-620 g/L, performing cooling and slicing in a drum-type slicer so as to obtain a sodium sulfide finished product with an iron content of less than 30 PPm and a content of 60%-62%. The method of the invention is applicable to any sodium sulfide production line. The invention has the characteristics of simple process, high production efficiency, less steam consumption, cleanness, environmental protection, etc.
Description
Technical field
The invention belongs to the sodium sulphite production field, particularly a kind of iron level is lower than the sodium sulphite production method of 30ppm.
Background technology
The sodium sulphite production process, entering of iron mainly appears at following operation: (1) sulfide black-ash thermalization operation (280g/L～310g/L sodium sulphite suspension liquid).(2) sodium sulphite clear liquid evaporization process.At present evaporation equipment has been the stainless steel plate type vaporizer, has solved entering of iron in the evaporization process.Sodium Sulphide clear liquid sedimentation deironing is one very important critical process in the sodium sulphite deferrization process.Current sodium sulphite suspension liquid sedimentation 24 hours can iron level be controlled at about 70PPm～150PPm in the sodium sulphite finished product with having now.
According to " sodium sulphite deironing mechanism " source investigation result, behind the sodium sulphite clear liquid thin up of 280g/L～300g/L, find to have the FeS precipitation to produce, but do like this, certainly will increase the evaporation cost, influence production efficiency.Carry out evaporation concentration as containing the sedimentary sodium sulphite diluent of FeS, along with improving constantly of sodium sulfide solution concentration, the FeS throw out begins dissolving on the contrary, when sodium sulfide content in the solution reaches 280g/L when above, the FeS throw out all dissolves, and the sodium sulphite clear liquid returns to dark red vitreous state again.So, want to make in the sodium sulphite product iron level to reduce to below the 30PPm, must change in the above sodium sulphite clear liquid of 280g/L between the FeS colloidal solid state of repulsion mutually, just can make the phase mutual coagulation of FeS micelle and precipitate.Although the sodium sulphite suspension liquid was through sedimentation deironing in 16～24 hours at present, iron level still within the scope of 0.03g/L～0.04g/L, continues the production problem that the prolongation settling time can't solve the following sodium sulphite of 30PPm in the above sodium sulphite clear liquid of 280g/L.Reason is as follows: thick sodium sulphite grog leaches through thermalization; gained sodium sulphite suspension liquid; after sedimentation; gained Sodium Sulphide clear liquid concentration is about 300g/L, and part FeS particulate forms micelle as the HS-ion in the glue nuclear absorption clear liquid and electronegative; these electronegative micelles are mutually exclusive; be difficult for cohesion, can't sedimentation, make the major cause that iron level increases in the sodium sulphite clear liquid.It is minimum to add the solubleness of FeS in water, is in metastable state.Therefore, as long as change the state of the charged negative FeS of solution, destroy its stability, iron just precipitates with the FeS form, but will suit industrialization reality.
Domestic sodium sulphite producer adds zinc salt or barium sulfide solution and produces the low iron sodium sulfide technology in the sodium sulphite clear liquid, and the shortcoming that adds zinc salt is zinc sulphide and the Iron sulfuret co-precipitation that generates, and its technical process is long, complicated operation; Add barium sulfide solution, not only additive decrementation steam, and the barium salt that generates precipitation effluxes, and constitutes second environmental pollution.
Summary of the invention
The object of the invention provides the sodium sulphite production method that a kind of iron level is lower than 30ppm, to solve long, the problem of environment pollution caused of the existing domestic technical process that utilizes zinc salt or barium sulphide deironing to produce low iron sodium sulfide.
The present invention includes the following step:
A, batching
Getting mass percent concentration and be 0.1%～0.2% the cationic polyacrylamide aqueous solution mixes 1:100～300 with the sodium sulphite clear liquid by volume as flocculation agent; The content of sodium sulphite is 275～310g/L in the sodium sulphite clear liquid, and cationic polyacrylamide (CPAM, molecular weight 5,000,000～1,000 ten thousand) is purchased in Xinxiang City, Henan Province Shunchang chemical industry company limited;
B, insulated and stirred
With A step mixed solution, under 50 ℃～60 ℃ heat-retaining condition, press 10r/min～20r/min stirring velocity, stirred 30 minutes～90 minutes;
C, filtration
Remove by filter the Iron sulfuret clay through flame filter press, get the low iron sodium sulfide clear liquid;
D, evaporation
The low iron sodium sulfide clear liquid of 275g/L～310g/L is squeezed into stainless steel plate type falling-film evaporator (existing installation), and to be evaporated to sodium sulfide content be the dense saltwater brine of 600g/L～620g/L; Vapor pressure is 0.38Mpa～0.4Mpa, 128 ℃～130 ℃ of vaporization temperatures, and vacuum tightness is 0.05Mpa～0.07Mpa;
E, finished product
With sodium sulfide content is that the dense saltwater brine of 600g/L～620g/L is put into the cooling section of drum-type slicing machine, and institute's final product is below the iron level 30PPm, and sodium sulfide content is at 60%～62% Sodium Sulfide Flakes finished product.
The principle of the invention be coal at 1050 ℃～1150 ℃ reduction of mirabilite, gained sodium sulphite grog leaches through thermalization.The gained sodium sulfide content is incubated sedimentations 24 hours at the suspension liquid of 275g/l～310g/l at 60 ℃～70 ℃, adds 0.1%～0.2% cationic polyacrylamide aqueous solution in the gained sodium sulphite clear liquid; Condense charged negative Iron sulfuret colloidal particle.The cationic polyacrylamide aqueous solution and sodium sulphite clear liquid volume ratio 1:100～300.Under 50 ℃～60 ℃ heat-retaining conditions, mixing speed 10～20r/min stirs after 30 minutes～90 minutes, and through plate filter, gained low iron sodium sulfide clear liquid is delivered to board-like stainless steel falling-film evaporator evaporation.At vapor pressure 0.38Mpa～0.4Mpa, 128 ℃～130 ℃ of vaporization temperatures, vacuum tightness 0.05Mpa～0.07Mpa evaporation.When being evaporated to sodium sulfide content and being the dense saltwater brine of 600g/L～620g/L, dope halogen is put into the drum-type slicing machine, feeding water cooling section, the gained sodium sulfide content is reduced to below the 30PPm more than the 70PPm of iron level by former technology in 60%～62% sodium sulphite finished product.
Cationic polyacrylamide (CPAM) is a chain macromolecule compound, because it has multiple active group, and can, absorption formation hydrogen bond affine with many materials.It mainly is the electronegative colloid of flocculation, have turbidity removal, decolouring, absorption, function such as bonding, be applicable to the higher wastewater treatments of industry organic colloid content such as dyeing, papermaking, food, building, metallurgy, ore dressing, coal dust, oil field, aquatic products processing and fermentation, be specially adapted to the processed of municipal effluent, municipal sludge, paper mill sludge and other industrial sludge.Therefore, add 0.1%～0.2% cationic polyacrylamide aqueous solution, can eliminate the electronegativity of FeS micelle particulate in the sodium sulphite clear liquid of the 300g/L left and right sides, absorption FeS colloidal particle form co-precipitation, reach the purpose of sodium sulphite finished product deironing, broken through domestic sodium sulphite producer's adding zinc salt or barium sulfide solution and produced the low iron sodium sulfide technology.
The inventive method can be used in any sodium sulphite production line.It is simple to have technology, the production efficiency height, and it is few to consume steam, characteristics such as clean environment firendly.
Embodiment
The following examples can make the present invention of those skilled in the art complete understanding, but do not limit the present invention in any way.
Embodiment 1:
Getting mass percent concentration is that 0.1% cationic polyacrylamide (molecular weight 5,000,000) 1L mixes with sodium sulphite clear liquid 100L, 50 ℃ of insulated and stirred 30 minutes, mixing speed 10r/min removes the Iron sulfuret clay through Plate Filtration and gets the low iron sodium sulfide clear liquid of sodium sulfide content at 312g/L; The low iron sodium sulfide clear liquid is squeezed into stainless steel plate type falling-film evaporator (existing installation) evaporation, when the low iron sodium sulfide clear liquid is evaporated to the dense saltwater brine that content is 600g/L, put into drum-type slicing machine water flowing cooling section, gained sodium sulphite finished product sodium sulfide content after testing is 60%, and iron level is 25PPm.Plate-type evaporator processing parameter: vapor pressure 0.38Mpa, 128 ℃ of vaporization temperatures, vacuum tightness 0.05Mpa.In the present embodiment in sodium sulphite liquid and the sodium sulphite finished product sodium sulphite main ingredient see the following form.
Table 1 sodium sulphite main ingredient
| The title project | Na 2S | Na 2CO 3 | Na 2S 2O 3 | Na 2SO 3 | Fe | Water-insoluble |
| Sodium sulphite clear liquid g.L -1 | 310 | 0.912 | 13.10 | 0.234 | 0.076 | ? |
| Low iron sodium sulfide clear liquid g.L -1 | 312 | 0.956 | 13.296 | 0.312 | 0.00132 | ? |
| Sodium sulphite finished product w% | 60% | 2.10% | 3.726% | 0.094% | 0.0025% | 0.051% |
Embodiment 2:
Getting mass percent concentration is that 0.1% cationic polyacrylamide (molecular weight 6,000,000) 1L mixes with the clear liquid 200L of sodium sulfide content at 275.275g/L, 60 ℃ of insulated and stirred 60 minutes, mixing speed 15r/min, remove the Iron sulfuret clay through Plate Filtration and get low iron sodium sulfide clear liquid 175L, when the low iron sodium sulfide clear liquid is squeezed into stainless steel plate type falling-film evaporator (existing installation) and is evaporated to content and is the dense saltwater brine of 610g/L, put into drum-type slicing machine water flowing cooling section, gained sodium sulphite finished product sodium sulfide content after testing is 61%, and iron level is 30PPm.Plate-type evaporator technical parameter: vapor pressure 0.4Mpa, 130 ℃ of vaporization temperatures, vacuum tightness 0.06Mpa.In the present embodiment in sodium sulphite liquid and the sodium sulphite finished product sodium sulphite main ingredient see the following form.
Table 2 sodium sulphite main ingredient
| The title project | Na 2S | Na 2CO 3 | Na 2S 2O 3 | Na 2SO 3 | Fe |
| Sodium sulphite clear liquid g.L -1 | 275.275 | 12.738 | 10.75 | 0.49 | 0.045 |
| Low iron sodium sulfide clear liquid g.L -1 | 301.092 | 13.882 | 10.11 | 0.51 | 0.015 |
| Sodium sulphite finished product w% | 61% | 1.8% | 3.441% | 0.08% | 0.0030% |
Embodiment 3:
Getting mass percent concentration is that 0.2% cationic polyacrylamide (molecular weight 8,000,000) 1L mixes with sodium sulphite clear liquid 300L, 55 ℃ of insulated and stirred 90 minutes, mixing speed 20r/min removes the Iron sulfuret clay through Plate Filtration, low iron sodium sulfide clear liquid 285L; When the low iron sodium sulfide clear liquid is squeezed into stainless steel plate type falling-film evaporator (existing installation) and is evaporated to content and is the dense saltwater brine of 620g/L, put into drum-type slicing machine water flowing cooling, section; Gained sodium sulphite finished product sodium sulfide content after testing is 62%, iron level 23PPm.Stainless steel plate type falling-film evaporator main technologic parameters: vapor pressure 0.38Mpa, 128 ℃ of vaporization temperatures, vacuum tightness 0.07Mpa.In the present embodiment in sodium sulphite liquid and the sodium sulphite finished product sodium sulphite main ingredient see the following form.
Table 3 sodium sulphite main ingredient
| The title project | Na 2S | Na 2CO 3 | Na 2S 2O 3 | Na 2SO 3 | Fe |
| Sodium sulphite clear liquid g.L -1 | 300 | 12.738 | 10.75 | 0.49 | 0.050 |
| Low iron sodium sulfide clear liquid g.L -1 | 302 | 12.179 | 11.011 | 0.481 | 0.011 |
| Sodium sulphite finished product w% | 62% | 1.71% | 3.207% | 0.077% | 0.0023% |
Embodiment 4
Getting mass percent concentration is that 0.2% cationic polyacrylamide (molecular weight 1,000 ten thousand) 1L mixes with sodium sulphite clear liquid 200L, 60 ℃ of insulated and stirred 60 minutes, mixing speed 20r/min removes the Iron sulfuret clay through Plate Filtration, gets low iron sodium sulfide clear liquid 175L; When the low iron sodium sulfide clear liquid is squeezed into stainless steel plate type falling-film evaporator (existing installation) and is evaporated to content and is the dense saltwater brine of 605g/L, put into drum-type slicing machine water flowing cooling, section; Gained sodium sulphite finished product sodium sulfide content after testing is 60.5%, iron level 10PPm.Stainless steel plate type falling-film evaporator main technologic parameters: vapor pressure 0.4Mpa, 130 ℃ of vaporization temperatures, vacuum tightness 0.06Mpa.In the present embodiment in sodium sulphite liquid and the sodium sulphite finished product sodium sulphite main ingredient see the following form.
Table 4 sodium sulphite main ingredient
| The title project | Na 2S | Na 2CO 3 | Na 2S 2O 3 | Na 2SO 3 | Fe |
| Sodium sulphite clear liquid g.L -1 | 290 | 12.738 | 10.75 | 0.49 | 0.045 |
| Low iron sodium sulfide clear liquid g.L -1 | 295 | 12.154 | 11.129 | 0.487 | 0.0005 |
| Sodium sulphite finished product w% | 60.5% | 1.77% | 3.21% | 0.07% | 0.0010% |
Claims (1)
1. an iron level is lower than the sodium sulphite production method of 30ppm, it is characterized in that it comprises the following steps:
A, batching
Getting mass percent concentration and be 0.1%～0.2% the cationic polyacrylamide aqueous solution mixes 1:100～300 with the sodium sulphite clear liquid of 280g/L～300g/L by volume as flocculation agent, the molecular weight of cationic polyacrylamide is 5,000,000～1,000 ten thousand, and the content of sodium sulphite is 275～310g/L in the sodium sulphite clear liquid;
B, insulated and stirred
With A step mixed solution, under 50 ℃～60 ℃ heat-retaining condition, press 10r/min～20r/min stirring velocity, stirred 30 minutes～90 minutes;
C, filtration
Remove by filter the Iron sulfuret clay through flame filter press, obtain the low iron sodium sulfide clear liquid;
D, evaporation
The low iron sodium sulfide clear liquid is squeezed into the evaporation of stainless steel plate type falling-film evaporator, and vapor pressure is 0.38Mpa～0.4Mpa, 128 ℃～130 ℃ of vaporization temperatures, and vacuum tightness is 0.05Mpa～0.07Mpa;
E, finished product
When the low iron sodium sulfide clear liquid is evaporated to sodium sulfide content and is the dense saltwater brine of 600g/L～620g/L, enter drum-type slicing machine cooling section, institute's final product is iron level at the following sodium sulphite finished product of 30PPm.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201110190518A CN102267689B (en) | 2011-07-08 | 2011-07-08 | Production method of sodium sulfide with iron content of less than 30 ppm |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201110190518A CN102267689B (en) | 2011-07-08 | 2011-07-08 | Production method of sodium sulfide with iron content of less than 30 ppm |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN102267689A true CN102267689A (en) | 2011-12-07 |
| CN102267689B CN102267689B (en) | 2012-10-03 |
Family
ID=45050175
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201110190518A Active CN102267689B (en) | 2011-07-08 | 2011-07-08 | Production method of sodium sulfide with iron content of less than 30 ppm |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN102267689B (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106185839A (en) * | 2016-07-01 | 2016-12-07 | 深州嘉信化工有限责任公司 | A kind of production method of ultralow ferrum industrial sodium sulfide |
| CN108002351A (en) * | 2016-10-31 | 2018-05-08 | 中国石油化工股份有限公司 | A kind of method of industrial goods purifying of sodium sulfide |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1244493A (en) * | 1999-09-13 | 2000-02-16 | 甘肃亚盛盐化工业集团有限责任公司 | Production technology of yellow flaky sodium sulfide with low carbon and iron contents |
| US7125497B1 (en) * | 2003-05-22 | 2006-10-24 | Sandia Corporation | Reactive formulations for a neutralization of toxic industrial chemicals |
-
2011
- 2011-07-08 CN CN201110190518A patent/CN102267689B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1244493A (en) * | 1999-09-13 | 2000-02-16 | 甘肃亚盛盐化工业集团有限责任公司 | Production technology of yellow flaky sodium sulfide with low carbon and iron contents |
| US7125497B1 (en) * | 2003-05-22 | 2006-10-24 | Sandia Corporation | Reactive formulations for a neutralization of toxic industrial chemicals |
Non-Patent Citations (1)
| Title |
|---|
| 《无机盐工业》 19861231 蒋杰明 硫化钠悬浊液加聚丙烯酰胺处理的研究 第15-17页 1 , 第6期 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106185839A (en) * | 2016-07-01 | 2016-12-07 | 深州嘉信化工有限责任公司 | A kind of production method of ultralow ferrum industrial sodium sulfide |
| CN108002351A (en) * | 2016-10-31 | 2018-05-08 | 中国石油化工股份有限公司 | A kind of method of industrial goods purifying of sodium sulfide |
Also Published As
| Publication number | Publication date |
|---|---|
| CN102267689B (en) | 2012-10-03 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN110482512A (en) | A kind of preparation method of battery-grade iron phosphate | |
| CN103739098B (en) | A kind of steel-making waste water conditioner | |
| CN107500393B (en) | Polyaluminum chloride-chitosan composite flocculant and preparation method and application thereof | |
| CN105036269B (en) | A kind of multiple-effect water treatment agent and preparation method thereof and method for treating water | |
| CN106517588B (en) | Efficient treatment method for graphene production wastewater | |
| CN108584901B (en) | Method for recovering ceramic-grade iron phosphate from polymetallic hazardous wastes | |
| JP6078379B2 (en) | Silica-containing water treatment apparatus, water treatment system, and silica-containing water treatment method | |
| CN105293728A (en) | Reagent used for treating papermaking waste water | |
| CN101948143A (en) | Method for preparing poly-silicate aluminum ferric chloride from fly ash | |
| CN101704570A (en) | Sewage treatment flocculating agent and using method thereof | |
| CN102267689B (en) | Production method of sodium sulfide with iron content of less than 30 ppm | |
| CN113401996A (en) | Water treatment defluorination medicament and preparation method thereof | |
| JP2011101830A (en) | Water treatment agent and water treatment method | |
| KR101980478B1 (en) | Manufacturing method of inorganic coagulants used acid waste water for treatment an activated clay | |
| CN102145946A (en) | Method for treating trace amount of cadmium in wastewater by chelation, coagulation and ultrafiltration combination | |
| CN112978994A (en) | Method for treating stainless steel pickling wastewater and synchronously synthesizing secondary iron mineral | |
| CN101955252B (en) | Method for extracting ferroaluminum from chemical sludge for preparing polyaluminum ferric chloride flocculating agent | |
| CN115745113B (en) | Coking wastewater defluorinating agent and application thereof | |
| CN103193342A (en) | Treatment process for preventing nonferrous smelting wastewater salt steaming crystallizing device from scaling | |
| CN112176346B (en) | Regenerant of phosphorus/sulfur mixed acid for chemical polishing, online regeneration method and system adopted by regenerant | |
| CN103657587A (en) | Preparation method of triazine ramification inserting layer laminated clay heavy metal catching agent and application | |
| CN113716665A (en) | Method for preparing flocculating agent by utilizing strong-acid wastewater containing phosphorus and sulfur | |
| CN106630293A (en) | Emergency treatment method for antimony-exceeded waste water at low temperature | |
| JP4271334B2 (en) | Sludge treatment method, organic wastewater treatment method including the treatment method, and organic wastewater treatment apparatus | |
| CN102225800B (en) | One-step reaction method for producing aluminum-zinc-magnesium multi-ion compound purifying agent |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant |