CN105819408A - Preparation method of barium thiosulfate - Google Patents
Preparation method of barium thiosulfate Download PDFInfo
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- CN105819408A CN105819408A CN201610154928.4A CN201610154928A CN105819408A CN 105819408 A CN105819408 A CN 105819408A CN 201610154928 A CN201610154928 A CN 201610154928A CN 105819408 A CN105819408 A CN 105819408A
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- CN
- China
- Prior art keywords
- filtrate
- barium
- sodium chloride
- hydrochloric acid
- filter cake
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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 compound preparation, and provides a preparation method of barium thiosulfate. The preparation method comprises the following steps: mixing oxidized filtrate of sulfurized dye and a diluted hydrochloric acid solution according to a mass ratio of 1:0.54 in a corrosion resistant container to carry out reactions; filtering the generated mixed solution of thiosulfuric acid and sodium chloride to obtain filter cake (impurity) and clarified filtrate; mixing clarified filtrate and barium chloride according to a mass ratio of 1:1.82 in a corrosion resistant container; and filtering the mixed solution containing generated barium thiosulfate, generated hydrochloric acid, and sodium chloride to obtain filter cake (barium thiosulfate) and filtrate containing sodium chloride. The oxidized filtrate of sulfurized dye is reutilized and effectively treated, the environment is protected, the preparation cost is reduced, and economic and social benefits are generated.
Description
Technical field
The invention belongs to field of compound preparation, particularly relate to the preparation method of a kind of Barium hyposulfite..
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) 19-21%;Sodium oxide 4%;Double sulphur black BRN 0.1-0.2%.
Prior art is prepared the relatively costly of Barium hyposulfite., and oxidation filtrate has harm to environment, owing to having the compound of economic worth containing five water sodium thiosulfate etc., cause the waste of resource if, with improper meeting.
Summary of the invention
Embodiments provide the preparation method of a kind of Barium hyposulfite., it is intended to solve the preparation cost of Barium hyposulfite. in prior art 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 Barium hyposulfite., described method comprise 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 barium chloride are reacted in corrosion-resistant container with the mass ratio of 1:1.82;
Filter the Barium hyposulfite. and hydrochloric acid and original sodium chloride mixed solution generated through described clear filtrate and barium chloride, obtain filter cake Barium hyposulfite. and the filtrate containing sodium chloride.
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 Barium hyposulfite. 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 barium chloride, again filter reacted solution and the hydrochloric acid solution of Barium hyposulfite. product, sodium chloride crystal and reusable edible can be arrived through suitable processing.
What Fig. 1 showed the preparation method of the Barium hyposulfite. 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 barium chloride are reacted in corrosion-resistant container with the mass ratio of 1:1.82;
In an embodiment of the present invention, clear filtrate mainly contains thiosulfuric acid and sodium chloride, and the chemical equation that thiosulfuric acid and barium chloride react is:
H2S2O3+BaCl2=BaS2O3+2HCl.
In step S104, filter clarified filtrate and the Barium hyposulfite. of barium chloride generation and hydrochloric acid and original sodium chloride mixed solution, obtain filter cake Barium hyposulfite. and the filtrate containing sodium chloride.
Its economic benefit can be increased by filter cake Barium hyposulfite. is carried out reworking, as a preferred embodiment of the present invention, can by scrubbed for filter cake Barium hyposulfite., dry, drying and crushing and check the weight and be packaged to be Barium hyposulfite. powder product.
Filtrate containing sodium chloride carries out deep processing to alleviate environmental pollution and increase social benefit, as a preferred embodiment of the present invention, filtrate containing sodium chloride is placed in decompression distillation in decompression distillator, through distilling, cool down, crystallize and be packaged to be sodium chloride crystal product and remaining distillating liquid.
In an embodiment of the present invention, remaining 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, having saved preparation cost, create economic benefit, also having 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 regarded as protection scope of the present invention.
Claims (5)
1. the preparation method of a Barium hyposulfite., 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 barium chloride are reacted in corrosion-resistant container with the mass ratio of 1:1.82;
Filter the Barium hyposulfite. and hydrochloric acid and original sodium chloride mixed solution generated through described clear filtrate and barium chloride, obtain filter cake Barium hyposulfite. and the filtrate containing sodium chloride.
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 filter cake Barium hyposulfite. after also include:
By scrubbed for described filter cake Barium hyposulfite., dry, drying and crushing and be packaged to be Barium hyposulfite. powder product.
4. the method for claim 1, it is characterised in that described in obtain the filtrate containing sodium chloride after also include:
The described filtrate containing sodium chloride is placed in decompression distillator, through distilling, cool down, crystallize and be packaged to be sodium chloride crystal product and remaining distillating liquid.
5. method as claimed in claim 4, it is characterised in that described remaining distillating liquid is mainly composed of hydrochloric acid solution, can be circulated utilization.
Priority Applications (1)
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CN201610154928.4A CN105819408A (en) | 2016-03-18 | 2016-03-18 | Preparation method of barium thiosulfate |
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CN201610154928.4A CN105819408A (en) | 2016-03-18 | 2016-03-18 | Preparation method of barium thiosulfate |
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2016
- 2016-03-18 CN CN201610154928.4A patent/CN105819408A/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: 20160803 |