CN105944678B - A kind of sodium hydrosulfide purification process - Google Patents
A kind of sodium hydrosulfide purification process Download PDFInfo
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- CN105944678B CN105944678B CN201610298034.2A CN201610298034A CN105944678B CN 105944678 B CN105944678 B CN 105944678B CN 201610298034 A CN201610298034 A CN 201610298034A CN 105944678 B CN105944678 B CN 105944678B
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- purification process
- nahs
- sodium hydrosulfide
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B17/00—Sulfur; Compounds thereof
- C01B17/22—Alkali metal sulfides or polysulfides
- C01B17/32—Hydrosulfides of sodium or potassium
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B17/00—Sulfur; Compounds thereof
- C01B17/22—Alkali metal sulfides or polysulfides
- C01B17/36—Purification
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2220/00—Aspects relating to sorbent materials
- B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
- B01J2220/44—Materials comprising a mixture of organic materials
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Analytical Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Separation Using Semi-Permeable Membranes (AREA)
- Agricultural Chemicals And Associated Chemicals (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
The invention belongs to purification processes technical fields, are related to a kind of sodium hydrosulfide purification process, and step includes：NaHS dissolves, and adds metal absorbent that impurity is precipitated, and double filtration dilutes, filling.The present invention can be such that the iron ion in sodium hydrosulfide is substantially reduced using the metal absorbent of special formulation, improve the quality of sodium hydrosulfide, shorten filtration time, also renewable, more environmentally friendly.
Description
Technical field
The present invention relates to purification processes technical field, more particularly to a kind of sodium hydrosulfide purification process.
Background technology
NaHS is mainly used for producing ammonium sulfide agriculture as a kind of basic chemical raw materials, the necessity of national economy
The raw material of medicine acetic acid alcohol semi-finished product, is largely used to flotation copper mine in mining industry, in leather industry for the defeathering of generation and
Tanning；For sloughing the free sulfur in activated carbon desulphurization agent in chemical fertilizer industry, contaminated for sulfurous acid in staple fibre production
Color is used for the synthesis of organic intermediate in dye industry and prepares the auxiliary agent of sulfur dye, for synthesizing in medical industry
The drugs such as cardiovascular diseases.With China's dye industry, leather industry, mining industry, chemical fertilizer industry, pharmaceuticals industry flourishing hair
The demand of exhibition and the support of national energy conservation and emission reduction policy, NaHS will be very big.Low iron NaHS is high added value
Product, with the recovery of China's economic in 2010, NaHS consumption figure constantly rises, in present world's dyestuff, organic pigment
The mesosome market focus is gradually shifted to Asia, and the kinds such as many intermediates such as phthalocyanine ketone, acetophenone amine intermediate are main
Asian countries is relied on, it is area that Asia, which has become the important production base of world's dyestuff, Pigment Intermediates and supply,.China is at present
The production of maximum NaHS and manufacturing nation in the world, but NaHS product is not top-quality product in the world, it is low
Iron NaHS color is plain, also has a certain distance from the market demand.With the increasing of the Chinese cotton goods export trade, sulphur
Change the dosage increase of dyestuff, printing and dyeing, ore dressing, chemical fertilizer, pharmaceutical industry to low iron NaHS, the low iron NaHS product in China will
There is the situation that supply falls short of demand.NaHS is vulcanizing agent and reducing agent of good performance.A variety of sulfide, great Su can be manufactured
It beats, be used as reducing agent in organic chemistry.It is widely used for chemical industry, pharmaceuticals industry, metallurgical industry and sewage disposal etc..
In recent years, each department is constantly increasing the demand of NaHS, past 5 years, and China's NaHS consumption increase rate is
10%, new requirement is also proposed for the quality of NaHS.As producing ammonium sulfide, sodium methyl mercaptide and pesticide ethyl mercaptan half
The raw material of finished product.Copper ore dressing is largely used in mining industry.With the defeathering of rawhide and tanning in leather industry.In chemical work
For sloughing the free sulfur in activated carbon desulphurization agent in industry.For sulfurous acid dyeing etc. in staple fibre production.It is important
Industrial chemicals and intermediate can synthesize Multiple Pesticides insecticide, fungicide, be occupied an important position in synthetic pesticide field.
It is used as vaccine adjuvant, this product that there are at low cost, stable components, have excellent performance, can be customized according to customer requirement in pharmaceutical synthesis
Different specifications (save the process that customer voluntarily prepares and purifies, and pack flexibly, is easy to use), largely can persistently supply
Feature can consolidate presence in the market with keen competition, and market occupancy volume steps up.
General iron ion content is very high (100ppm or more) in the commercially available NaHS of China at present, such NaHS
It is bad for industries reliabilities such as electronics, semiconductor, accuracy electroplate industry, chemical fibre, medicine.
The present invention is just to provide for a kind of new technology to solve the problems, such as that NaHS iron content is high.
Invention content
The main purpose of the present invention is to provide a kind of sodium hydrosulfide purification process.
The present invention is achieved through the following technical solutions above-mentioned purpose：A kind of sodium hydrosulfide purification process, step include：
1. NaHS is dissolved in deionized water；
2. 1-5wt% metal absorbents are added in step 1. acquired solution, 10min is stirred, so that impurity is precipitated, the gold
It includes 70-90wt% trithiocyanuric acids trisodium salt and the xanthate of surplus to belong to adsorbent,；
3. to step, 2. gained liquid is filtered using two-filtration devices；
4. by step, 3. acquired solution adds deionized water to be diluted to required concentration, filling.
Specifically, the xanthate is insoluble starch xantate.
Further, the mass percent of the trithiocyanuric acid trisodium salt is 80-90wt%.
Specifically, the two-filtration devices use ceramic membrane filter core.
Further, the two-filtration devices inner lining polypropylene resin.
Using above-mentioned technical proposal, the advantageous effect of technical solution of the present invention is：
1, the present invention can be such that the iron ion in sodium hydrosulfide is substantially reduced using the metal absorbent of special formulation,
Improve the quality of sodium hydrosulfide；
2, xanthate keeps precipitation loose, it is easier to filter, shorten filtration time, filter core frequency of maintenance reduces；
3, metal absorbent can regenerate use, more environmentally friendly；
4, filter device can be to avoid introducing other impurities metal ion.
Specific implementation mode
A kind of sodium hydrosulfide purification process of the application metal absorbent, step include：
1. NaHS is dissolved in deionized water；
2. 1-5wt% metal absorbents are added in step 1. acquired solution, 10min is stirred, so that impurity is precipitated, the gold
It includes 70-90wt% trithiocyanuric acids trisodium salt and the xanthate of surplus to belong to adsorbent,；
3. to step, 2. gained liquid is filtered using two-filtration devices；
4. by step, 3. acquired solution adds deionized water to be diluted to required concentration, filling.
With reference to specific embodiment, invention is further described in detail.
Embodiment 1：
1. NaHS is dissolved in deionized water；
2. 1wt% metal absorbents (trisodium containing trithiocyanuric acid in metal absorbent is added in step 1. acquired solution
Salt 90wt%, insoluble starch xantate 10wt%), 10min is stirred, impurity is made to be precipitated；
3. using, using acrylic resin as the ceramic membrane two-filtration devices of liner, to step, 2. gained liquid is filtered；
4. by step, 3. acquired solution adds deionized water to be diluted to required concentration, filling.
Metal absorbent can elute from the filter core of ceramic membrane two-filtration devices and regenerate use, more environmentally friendly.
Embodiment 2-7
By the method that each component mass percent specified in table 1 repeats EXPERIMENTAL EXAMPLE 1, different NaHSs is obtained
Refined solution.
Table 1：
NaHS refined solution obtained by the method for embodiment 1 is repeated using trithiocyanuric acid trisodium salt as metal absorbent to make
For reference examples, the final iron concentration and filtration time of detection record embodiment 1-7 and reference examples.
Table 2：
Xanthate can make trithiocyanuric acid trisodium salt have better adsorptivity to iron ion, can make the iron in solution
Ion concentration drops to 10ppm hereinafter, enabling the precipitation generated loose, and filtration time is made to be obviously shortened, and decreases filter element cleaning frequency
Rate, therefore the overall effect for being better than trithiocyanuric acid trisodium salt metal absorbent.
The regeneration capable of washing of ceramic membrane two-filtration devices, acrylic resin will not foul solution, will not especially introduce it
His metal impurities, it is ensured that the quality of final products.
Above-described is only some embodiments of the present invention.For those of ordinary skill in the art, not
Under the premise of being detached from the invention design, various modifications and improvements can be made, these belong to the protection model of the present invention
It encloses.
Claims (5)
1. a kind of sodium hydrosulfide purification process, it is characterised in that step includes：
1. NaHS is dissolved in deionized water；
2. 1-5wt% metal absorbents are added in step 1. acquired solution, 10min is stirred, impurity is made to be precipitated, the metal is inhaled
The attached dose of xanthate for including 70-90wt% trithiocyanuric acids trisodium salt and surplus；
3. to step, 2. gained liquid is filtered using two-filtration devices；
4. by step, 3. acquired solution adds deionized water to be diluted to required concentration, filling.
2. purification process according to claim 1, it is characterised in that：The xanthate is insoluble starch xanthic acid
Ester.
3. purification process according to claim 1 or 2, it is characterised in that：The quality hundred of the trithiocyanuric acid trisodium salt
Divide than being 80-90wt%.
4. purification process according to claim 1, it is characterised in that：It is characterized in that：The two-filtration devices use
Ceramic membrane filter core.
5. purification process according to claim 4, it is characterised in that：The two-filtration devices inner lining polypropylene resin.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201610298034.2A CN105944678B (en) | 2016-05-06 | 2016-05-06 | A kind of sodium hydrosulfide purification process |
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| CN201610298034.2A CN105944678B (en) | 2016-05-06 | 2016-05-06 | A kind of sodium hydrosulfide purification process |
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| CN105944678A CN105944678A (en) | 2016-09-21 |
| CN105944678B true CN105944678B (en) | 2018-07-13 |
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| CN109956456B (en) * | 2019-03-25 | 2022-05-06 | 山东益大新材料股份有限公司 | Method for purifying sodium hydrosulfide |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5006654A (en) * | 1987-08-31 | 1991-04-09 | Degussa Aktiengesellschaft | Method of preparing trisodium 2,4,6-mercapto-s-triazine nonahydrate |
| CN103351316A (en) * | 2013-07-12 | 2013-10-16 | 黄河三角洲京博化工研究院有限公司 | Method for removing iron ions from sodium thiomethoxide solution |
| CN103755067A (en) * | 2014-01-03 | 2014-04-30 | 上海丰信环保科技有限公司 | Treatment method for removing complex nickel out of wastewater |
| CN105463521A (en) * | 2016-01-07 | 2016-04-06 | 杭州东方表面技术有限公司 | Environment-friendly cyanide-free alkaline zinc plating purification additive |
-
2016
- 2016-05-06 CN CN201610298034.2A patent/CN105944678B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5006654A (en) * | 1987-08-31 | 1991-04-09 | Degussa Aktiengesellschaft | Method of preparing trisodium 2,4,6-mercapto-s-triazine nonahydrate |
| CN103351316A (en) * | 2013-07-12 | 2013-10-16 | 黄河三角洲京博化工研究院有限公司 | Method for removing iron ions from sodium thiomethoxide solution |
| CN103755067A (en) * | 2014-01-03 | 2014-04-30 | 上海丰信环保科技有限公司 | Treatment method for removing complex nickel out of wastewater |
| CN105463521A (en) * | 2016-01-07 | 2016-04-06 | 杭州东方表面技术有限公司 | Environment-friendly cyanide-free alkaline zinc plating purification additive |
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| CN105944678A (en) | 2016-09-21 |
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