CN105584995A - Preparation method of ammonium thiosulfate - Google Patents
Preparation method of ammonium thiosulfate Download PDFInfo
- Publication number
- CN105584995A CN105584995A CN201610154930.1A CN201610154930A CN105584995A CN 105584995 A CN105584995 A CN 105584995A CN 201610154930 A CN201610154930 A CN 201610154930A CN 105584995 A CN105584995 A CN 105584995A
- Authority
- CN
- China
- Prior art keywords
- sodium chloride
- ats
- ammonium
- filtrate
- ammonium thiosulphate
- 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.)
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Classifications
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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
- C01B17/64—Thiosulfates; Dithionites; Polythionates
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D3/00—Halides of sodium, potassium or alkali metals in general
- C01D3/04—Chlorides
- C01D3/06—Preparation by working up brines; seawater or spent lyes
Abstract
The invention is suitable for the field of compound preparation and provides a preparation method of ammonium thiosulfate. The method comprises the steps that oxidation filter liquor for vulcanizing dye and a hydrochloric acid dilute solution react in a corrosion-resistant container according to the mass ratio of 1:0.54; a thiosulfuric acid and sodium chloride mixed solution generated on the lower-temperature condition is filtered to obtain filter cake impurities and clarify filter liquor; the clarified filter liquor and ammonium chloride react in the corrosion-resistant container according to the mass ratio of 1:0.94; ammonium thiosulfate generated by the clarified filter liquor and ammonium chloride, hydrochloric acid and an original sodium chloride solution are filtered to obtain filter liquor containing ammonium thiosulfate and sodium chloride; the filter liquor containing ammonium thiosulfate and sodium chloride is obtained; the filter liquor containing ammonium thiosulfate and sodium chloride is placed into a pressure reduction distiller to obtain ammonium thiosulfate, sodium chloride and distilled liquid. The oxidation filter liquor for vulcanizing the dye is reutilized and effectively treated, environment is protected, preparation cost is saved, and economic benefits are created.
Description
Technical field
The invention belongs to compound preparation field, relate in particular to a kind of preparation method of ATS (Ammonium thiosulphate).
Background technology
Sulfur Black claims again to vulcanize unit or sulphur black, is the sulfur dye of consumption figure maximum. Owing to producing the different and user's of upper process conditions requirement, can make the different Sulfur Black of a variety of color and lusters, the sulphur black BN(green light of domestic production), BRN (blue or green ruddiness), RN(ruddiness), the kind such as BN is double, BRN is double.
It is to be raw material by dinitrochlorobenzene and NaOH that double sulphur black BRN is produced, through being hydrolyzed into 2,4-DNP sodium salt, with making through technical process such as air oxidation, filtration drying, drying and crushing after sodium polysulfide sulfuration again.
Oxidation filtrate comes from the filter process after oxidation, wherein, comprises the washings of filtration. The generation of oxidation filtrate is 3.2:1 with the generation of double sulphur black BRN ratio. 5000 tons/year of double sulphur black BRN production scales, the generation of oxidation filtrate is 1.6 ten thousand tons. The composition of oxidation filtrate: five water sodium thiosulfate (being commonly called as dodium thiosulfate or hypo) accounting is 19-21%; Sodium oxide molybdena accounts for 4%; Double sulphur black BRN accounts for 0.1-0.2%.
The cost of preparing ATS (Ammonium thiosulphate) in prior art is high, and oxidation filtrate has harm to environment, has the compound of economic worth, if utilize improper meeting to cause the waste of resource owing to containing five water sodium thiosulfate etc.
Summary of the invention
The embodiment of the present invention provides a kind of preparation method of ATS (Ammonium thiosulphate), and the preparation cost that is intended to solve ATS (Ammonium thiosulphate) of the prior art is high, and the harm of oxidation filtrate to environment, can not effectively utilize its economic worth to cause the problem of the wasting of resources.
The embodiment of the present invention is achieved in that a kind of preparation method of ATS (Ammonium thiosulphate), and described method comprises the steps:
The oxidation filtrate of sulfur dye and hydrochloric acid weak solution are reacted in corrosion-resistant container with the mass ratio of 1:0.54;
Filter the thiosulfuric acid and the sodium chloride mixed solution that under cryogenic conditions, are generated by oxidation filtrate and the hydrochloric acid weak solution of described sulfur dye, obtain filter cake impurity clear filtrate;
Described clear filtrate and ammonium chloride are reacted in corrosion-resistant container with the mass ratio of 1:0.94;
Filter ATS (Ammonium thiosulphate) and hydrochloric acid and original sodium chloride mixed solution through described clear filtrate and ammonium chloride generation, obtain the filtrate of containing ATS (Ammonium thiosulphate) and sodium chloride;
The described filtrate of containing ATS (Ammonium thiosulphate) and sodium chloride is placed in to decompression distillation device, obtains ATS (Ammonium thiosulphate), sodium chloride and distillating liquid.
The embodiment of the present invention is utilized again by the oxidation filtrate to sulfur dye, has effectively administered the oxidation filtrate of sulfur dye and has protected environment, saves preparation cost, has created economic benefit, has also embodied plentiful and substantial social benefit simultaneously.
Brief description of the drawings
Fig. 1 represents the preparation method's of the ATS (Ammonium thiosulphate) that the embodiment of the present invention provides realization flow figure.
Detailed description of the invention
In order to make object of the present invention, technical scheme and advantage clearer, below in conjunction with drawings and Examples, the present invention is further elaborated. Should be appreciated that specific embodiment described herein, only in order to explain the present invention, is not intended to limit the present invention.
The embodiment of the present invention is by reacting the oxidation filtrate of sulfur dye with hydrochloric acid weak solution, and filter reacted solution, it is reacted with ammonium chloride, again filter reacted solution and pass through suitable processing the hydrochloric acid solution that can arrive ATS (Ammonium thiosulphate), sodium chloride crystal and reusable edible.
Fig. 1 shows the preparation method's of the ATS (Ammonium thiosulphate) that the embodiment of the present invention provides realization flow, and details are as follows:
In step S101, the oxidation filtrate of sulfur dye and hydrochloric acid weak solution are reacted in corrosion-resistant container with the mass ratio of 1:0.54;
In an embodiment of the present invention, the oxidation filtrate of sulfur dye, taking sodium thiosulfate as main component, contains a small amount of sodium oxide molybdena.
The oxidation filtrate of sulfur dye and the hydrochloric acid solution chemical equation reacting in corrosion-resistant container is:
Na2S2O3+2HCl=2NaCl+H2S2O3;
Na2O+2HCl=2NaCl+H2O.
In step S102, filter the thiosulfuric acid and the sodium chloride mixed solution that under cryogenic conditions, are generated by oxidation filtrate and the hydrochloric acid weak solution of sulfur dye, obtain filter cake impurity clear filtrate;
In an embodiment of the present invention, the filter cake impurity obtaining can be processed through modes such as buried or burnings.
In step S103, clear filtrate and ammonium chloride are reacted in corrosion-resistant container with the mass ratio of 1:0.94;
In an embodiment of the present invention, clear filtrate mainly contains thiosulfuric acid and sodium chloride, and the chemical equation that thiosulfuric acid and ammonium chloride react is:
H2S2O3+2NH4Cl=(NH4)2S2O3+2HCl.
In step S104, filter ATS (Ammonium thiosulphate) and hydrochloric acid and original sodium chloride mixed solution through clear filtrate and ammonium chloride generation, obtain the filtrate of containing ATS (Ammonium thiosulphate) and sodium chloride;
After filtering the ATS (Ammonium thiosulphate) that generates through clear filtrate and ammonium chloride and hydrochloric acid and original sodium chloride mixed solution, can produce a small amount of filter cake impurity, in an embodiment of the present invention, by a small amount of filter cake impurity burning or buried.
In step S105, the filtrate of containing ATS (Ammonium thiosulphate) and sodium chloride is placed in to decompression distillation device, obtain ATS (Ammonium thiosulphate), sodium chloride and distillating liquid.
By ATS (Ammonium thiosulphate) and sodium chloride are again processed and can be increased its economic benefit, as a preferred embodiment of the present invention, ATS (Ammonium thiosulphate) and sodium chloride are drawn to ATS (Ammonium thiosulphate) and sodium chloride crystal product through crystallisation by cooling, crushing packing.
In an embodiment of the present invention, distillating liquid main component is hydrochloric acid solution, can recycle. So not only can saving resource, and promote economic benefit.
The embodiment of the present invention is utilized again by the oxidation filtrate to sulfur dye, has effectively administered the oxidation filtrate of sulfur dye and has protected environment, saves preparation ATS (Ammonium thiosulphate) cost, has created economic benefit, has also embodied plentiful and substantial social benefit simultaneously.
The above is only the preferred embodiment of the present invention; it should be pointed out that for those skilled in the art, under the premise without departing from the principles of the invention; can also make some improvements and modifications, these improvements and modifications also should be considered as protection scope of the present invention.
Claims (4)
1. a preparation method for ATS (Ammonium thiosulphate), is characterized in that, described method comprises the steps:
The oxidation filtrate of sulfur dye and hydrochloric acid weak solution are reacted in corrosion-resistant container with the mass ratio of 1:0.54;
Filter the thiosulfuric acid and the sodium chloride mixed solution that under cryogenic conditions, are generated by oxidation filtrate and the hydrochloric acid weak solution of described sulfur dye, obtain filter cake impurity clear filtrate;
Described clear filtrate and ammonium chloride are reacted in corrosion-resistant container with the mass ratio of 1:0.94;
Filter ATS (Ammonium thiosulphate) and hydrochloric acid and original sodium chloride mixed solution through described clear filtrate and ammonium chloride generation, obtain the filtrate of containing ATS (Ammonium thiosulphate) and sodium chloride;
The described filtrate of containing ATS (Ammonium thiosulphate) and sodium chloride is placed in to decompression distillation device, obtains ATS (Ammonium thiosulphate), sodium chloride and distillating liquid.
2. the method for claim 1, is characterized in that, the oxidation filtrate of described sulfur dye is taking sodium thiosulfate as main component.
3. the method for claim 1, is characterized in that, described in obtain also comprising after ATS (Ammonium thiosulphate), sodium chloride:
Described ATS (Ammonium thiosulphate), sodium chloride are drawn to ATS (Ammonium thiosulphate) and sodium chloride crystal product through crystallisation by cooling, crushing packing.
4. the method for claim 1, is characterized in that, described distillating liquid main component is hydrochloric acid solution, can recycle.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610154930.1A CN105584995A (en) | 2016-03-18 | 2016-03-18 | Preparation method of ammonium thiosulfate |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610154930.1A CN105584995A (en) | 2016-03-18 | 2016-03-18 | Preparation method of ammonium thiosulfate |
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| CN105584995A true CN105584995A (en) | 2016-05-18 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN201610154930.1A Pending CN105584995A (en) | 2016-03-18 | 2016-03-18 | Preparation method of ammonium thiosulfate |
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101850952A (en) * | 2010-05-14 | 2010-10-06 | 青岛楚天节能技术有限公司 | Production technique for extracting ammonium thiosulfate and ammonium thiocyanate from desulfurization waste liquor |
| CN103213953A (en) * | 2012-01-20 | 2013-07-24 | 鞍钢集团工程技术有限公司 | Technology for extracting ammonium thiosulfate and ammonium thiocyanate by desulphurization waste liquid |
-
2016
- 2016-03-18 CN CN201610154930.1A patent/CN105584995A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101850952A (en) * | 2010-05-14 | 2010-10-06 | 青岛楚天节能技术有限公司 | Production technique for extracting ammonium thiosulfate and ammonium thiocyanate from desulfurization waste liquor |
| CN103213953A (en) * | 2012-01-20 | 2013-07-24 | 鞍钢集团工程技术有限公司 | Technology for extracting ammonium thiosulfate and ammonium thiocyanate by desulphurization waste liquid |
Non-Patent Citations (3)
| Title |
|---|
| WIKI: "《Wikipedia》", 31 December 1957 * |
| 网络: "《盐酸与硫代硫酸钠的探究实验》", 《盐酸与硫代硫酸钠的探究实验》 * |
| 郭德威 等: "《无机化学丛书》", 31 March 2011 * |
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Application publication date: 20160518 |
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