CN105836714A - Preparation method of zinc thiosulfate - Google Patents
Preparation method of zinc thiosulfate Download PDFInfo
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- CN105836714A CN105836714A CN201610178643.4A CN201610178643A CN105836714A CN 105836714 A CN105836714 A CN 105836714A CN 201610178643 A CN201610178643 A CN 201610178643A CN 105836714 A CN105836714 A CN 105836714A
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- China
- Prior art keywords
- filtrate
- sodium chloride
- zinc
- thiosulfuric acid
- acid zinc
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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
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention belongs to the field of preparation of compounds and provides a preparation method of zinc thiosulfate. The preparation method includes the following steps: 1) performing a reaction to an oxidized filtrate of a sulfurized dye and a diluted hydrochloric acid solution according to the mass ratio of 1:0.54 in a corrosion-resistant container; 2) filtering the mixed solution of thiosulfuric acid and sodium chloride, which is generated at the low temperature, to obtain cake impurity and a clear filtrate; 3) performing a reaction to the clear filtrate and zinc chloride according to the mass ratio of 1:1.19 in a corrosion-resistant container; 4) filtering the mixed solution composed of zinc thiosulfate and the hydrochloric acid, which is generated from the clear filtrate and the zinc chloride, and the original sodium chloride to obtain the filtrate containing zinc thiosulfate and sodium chloride; and 5) performing reduced-pressure distillation in a reduced-pressure distiller to the filtrate containing the zinc thiosulfate and sodium chloride to obtain the zinc thiosulfate, the sodium chloride and distilled liquid. The oxidized filtrate of the sulfurized dye is recycled in the invention, so that the oxidized filtrate is treated effectively, thereby protecting environment, saving preparation cost and creating economic benefit.
Description
Technical field
The invention belongs to field of compound preparation, particularly relate to the preparation method of a kind of thiosulfuric acid zinc.
Background technology
Sulfur Black, also known as sulfuration unit or sulphur black, is the sulfur dye of consumption figure maximum.Owing to producing, upper process conditions are different and the requirement of user, can prepare the Sulfur Black that a variety of color and luster is different, the sulphur black BN(green light of domestic production), BRN (blue or green HONGGUANG), RN(HONGGUANG), the kind such as BN is double, BRN is double.
It is to be raw material by dinitrochlorobenzene and sodium hydroxide that double sulphur black BRN produces, through being hydrolyzed into 2,4-DNP sodium salt, after vulcanizing with sodium polysulphide again through air oxidation, filter the technical processs such as drying, drying and crushing and prepare.
Oxidation filtrate comes from the filter process after oxidation, wherein, including the washings filtered.The generation amount of oxidation filtrate and the generation amount of double sulphur black BRN are than for 3.2:1.Double sulphur black BRN production scale 5000 tons/year, the generation amount of oxidation filtrate is 1.6 ten thousand tons.The composition of oxidation filtrate: five water sodium thiosulfate (being commonly called as sodium hyposulfite or hypo) accounting is 19-21%；Sodium oxide accounts for 4%；Double sulphur black BRN accounts for 0.1-0.2%.
The cost preparing thiosulfuric acid zinc in prior art is high, and oxidation filtrate has harm to environment, is the most well utilized, and owing to having the compound of economic worth containing five water sodium thiosulfate etc., causes the waste of resource if, with improper meeting.
Summary of the invention
Embodiments provide the preparation method of a kind of thiosulfuric acid zinc, it is intended to the preparation cost solving thiosulfuric acid zinc of the prior art is high, and oxidation filtrate to the harm of environment, can not effectively utilize the problem that its economic worth causes the wasting of resources.
The embodiment of the present invention is achieved in that the preparation method of a kind of thiosulfuric acid zinc, 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 sodium chloride mixed solution generated with hydrochloric acid weak solution by the oxidation filtrate of described sulfur dye under cryogenic conditions, obtain filter cake impurity clear filtrate；
Described clear filtrate and zinc chloride are reacted in corrosion-resistant container with the mass ratio of 1:1.19；
Filter the thiosulfuric acid zinc and hydrochloric acid and original sodium chloride mixed solution generated through described clear filtrate and zinc chloride, obtain the filtrate containing thiosulfuric acid zinc and sodium chloride；
The described filtrate containing thiosulfuric acid zinc and sodium chloride is placed in decompression distillator, obtains thiosulfuric acid zinc, sodium chloride and distillating liquid.
The embodiment of the present invention by the oxidation filtrate of sulfur dye is carried out again with, effectively administered the oxidation filtrate of sulfur dye and protected environment, having saved preparation cost, create economic benefit, also having embodied plentiful and substantial social benefit simultaneously.
Accompanying drawing explanation
Fig. 1 represents the flowchart of the preparation method of the thiosulfuric acid zinc that the embodiment of the present invention provides.
Detailed description of the invention
In order to make the purpose 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, make it react with zinc chloride, again filter reacted solution and the hydrochloric acid solution of thiosulfuric acid zinc, sodium chloride crystal and reusable edible can be arrived through suitable processing.
What Fig. 1 showed the preparation method of the thiosulfuric acid zinc that the embodiment of the present invention provides realizes flow process, 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 is with sodium thiosulfate as main component, containing small amounts sodium.
The oxidation filtrate of sulfur dye and the hydrochloric acid solution chemical equation reacted in corrosion-resistant container is:
Na2S2O3+2HCl=2NaCl+H2S2O3;
Na2O+2HCl=2NaCl+H2O.
In step s 102, filter the thiosulfuric acid and sodium chloride mixed solution generated with hydrochloric acid weak solution by the oxidation filtrate of sulfur dye under cryogenic conditions, obtain filter cake impurity clear filtrate；
In an embodiment of the present invention, the filter cake impurity obtained can process through modes such as buried or burnings.
In step s 103, clear filtrate and zinc chloride are reacted in corrosion-resistant container with the mass ratio of 1:1.19；
In an embodiment of the present invention, clear filtrate mainly contains thiosulfuric acid and sodium chloride, and the chemical equation that thiosulfuric acid and zinc chloride react is:
H2S2O3+ZnCl2=
ZnS2O3+2HCl.
In step S104, filter clarified filtrate and the thiosulfuric acid zinc of zinc chloride generation and hydrochloric acid and original sodium chloride mixed solution, obtain the filtrate containing thiosulfuric acid zinc and sodium chloride；
A small amount of filter cake impurity can be produced after filtering clarified filtrate and the thiosulfuric acid zinc of zinc chloride generation and hydrochloric acid and original sodium chloride mixed solution, in an embodiment of the present invention, a small amount of filter cake impurity is burned or buried.
In step S105, the filtrate containing thiosulfuric acid zinc and sodium chloride is placed in decompression distillator, obtains thiosulfuric acid zinc, sodium chloride and distillating liquid.
Its economic benefit can be increased by thiosulfuric acid zinc and sodium chloride are carried out reworking, as a preferred embodiment of the present invention, thiosulfuric acid zinc and sodium chloride be drawn thiosulfuric acid zinc and sodium chloride crystal product through crystallisation by cooling, crushing packing.
In an embodiment of the present invention, distillating liquid is mainly composed of hydrochloric acid solution, can be circulated utilization.So it is possible not only to save resource, and promotes economic benefit.
The embodiment of the present invention by the oxidation filtrate of sulfur dye is carried out again with, effectively administered the oxidation filtrate of sulfur dye and protected environment, thiosulfuric acid zinc cost is prepared in saving, creates economic benefit, also embodies 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 regarded as protection scope of the present invention.
Claims (4)
1. the preparation method of a thiosulfuric acid zinc, it is characterised 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 sodium chloride mixed solution generated with hydrochloric acid weak solution by the oxidation filtrate of described sulfur dye under cryogenic conditions, obtain filter cake impurity clear filtrate；
Described clear filtrate and zinc chloride are reacted in corrosion-resistant container with the mass ratio of 1:1.19；
Filter the thiosulfuric acid zinc and hydrochloric acid and original sodium chloride mixed solution generated through described clear filtrate and zinc chloride, obtain the filtrate containing thiosulfuric acid zinc and sodium chloride；
The described filtrate containing thiosulfuric acid zinc and sodium chloride is placed in decompression distillator, obtains thiosulfuric acid zinc, sodium chloride and distillating liquid.
2. the method for claim 1, it is characterised in that the oxidation filtrate of described sulfur dye is with sodium thiosulfate as main component.
3. the method for claim 1, it is characterised in that described in obtain thiosulfuric acid zinc, sodium chloride after also include:
Described thiosulfuric acid zinc, sodium chloride are drawn thiosulfuric acid zinc and sodium chloride crystal product through crystallisation by cooling, crushing packing.
4. the method for claim 1, it is characterised in that described distillating liquid is mainly composed of hydrochloric acid solution, can be circulated utilization.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610178643.4A CN105836714A (en) | 2016-03-28 | 2016-03-28 | Preparation method of zinc thiosulfate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610178643.4A CN105836714A (en) | 2016-03-28 | 2016-03-28 | Preparation method of zinc thiosulfate |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN105836714A true CN105836714A (en) | 2016-08-10 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610178643.4A Pending CN105836714A (en) | 2016-03-28 | 2016-03-28 | Preparation method of zinc thiosulfate |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN105836714A (en) |
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2016
- 2016-03-28 CN CN201610178643.4A patent/CN105836714A/en active Pending
Non-Patent Citations (4)
| Title |
|---|
| 《化工百科全书》编辑委员会: "《化工百科全书》", 30 April 1996, 化学工业出版社 * |
| 吕述萍等: "《无机及分析化学实验》", 31 July 2013, 北京理工大学出版社 * |
| 戴安邦等: "《无机化学教程 上册》", 31 July 1959, 高等教育出版社 * |
| 郭德威等: "《无机化学丛书》", 31 March 2011, 科学出版社 * |
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Application publication date: 20160810 |
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