CN105819407A - Method of preparing thiosulfuric acid and sodium chloride from filtrate of vulcanized dye - Google Patents
Method of preparing thiosulfuric acid and sodium chloride from filtrate of vulcanized dye Download PDFInfo
- Publication number
- CN105819407A CN105819407A CN201610150810.4A CN201610150810A CN105819407A CN 105819407 A CN105819407 A CN 105819407A CN 201610150810 A CN201610150810 A CN 201610150810A CN 105819407 A CN105819407 A CN 105819407A
- Authority
- CN
- China
- Prior art keywords
- filtrate
- sodium chloride
- thiosulfuric acid
- dye
- vulcanized
- 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.)
- Pending
Links
Classifications
-
- 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
- C01D3/22—Preparation in the form of granules, pieces, or other shaped products
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a method of preparing thiosulfuric acid and sodium chloride from filtrate of vulcanized dye, and relates to the technical field of chemical waste comprehensive treatment and utilization in dye industry. The preparation method comprises the following steps: adding oxidized filtrate of vulcanized dye and a diluted hydrochloric acid solution into a reactor to carry out reactions so as to generate a mixed solution of thiosulfuric acid and sodium chloride; filtering the mixed solution, filling the filtrate into a reduced pressure distiller to carry out reduced pressure distillation, then cooling to carry out crystallization, washing the crystals, drying to obtain sodium chloride crystals; filling residual distillation liquid into a purifier, adding silver hydroxide to form silver chloride precipitate, filtering, adding calcium chloride into the residual sodium hydroxide solution to neutralize sodium hydroxide to obtain calcium hydroxide precipitate, filtering, and carrying out reduced pressure distillation and condensation to obtain a thiosulfuric acid liquid. The provided method is simple, prepares thiosulfuric acid and sodium chloride from waste oxidized filtrate, effectively treats and utilizes the oxidized filtrate of vulcanized dye, protects the environment, and saves the resources.
Description
Technical field
The present invention relates to dyestuff chemistry three industrial wastes comprehensive control and the technical field of utilization, be specifically related to a kind of method using sulfur dye filtrate to prepare thiosulfuric acid and sodium chloride.
Background technology
nullSulfur Black is also known as sulfuration unit or sulphur black，It it is the sulfur dye of consumption figure maximum，Owing to producing the different requirement with user of upper process conditions，The Sulfur Black that a variety of color and luster is different can be prepared，The sulphur black of domestic production is divided into BN(green light)、BRN (blue or green HONGGUANG)、RN(HONGGUANG)、BN is double、The multiple kinds such as BRN is double，It is to be raw material by dinitrochlorobenzene and sodium hydroxide that double sulphur black BRN produces，Through being hydrolyzed into 2,2, 4-dinitrophenol sodium salt，Again through air oxidation after vulcanizing with sodium polysulphide、Filter and dry、The technical processs such as drying and crushing and prepare，Double sulphur black BRN production process can produce a lot of oxidation filtrate，Oxidation filtrate is contained within the five water sodium thiosulfate of 19-21%，The sodium oxide of 4%，General factory is all to be drained as waste liquid by oxidation filtrate，Not only pollute the environment，But also the waste of resource can be caused.
Summary of the invention
It is an object of the invention to provide a kind of method using sulfur dye filtrate to prepare thiosulfuric acid and sodium chloride; its method is simple; discarded oxidation filtrate is re-used; prepare thiosulfuric acid and sodium chloride product; can effectively administer and make use of sulfur dye oxidation filtrate; not only protect environment, saved resource simultaneously, create good economic benefit.
nullIn order to solve the problem existing for background technology，The present invention is by the following technical solutions: the oxidation filtrate of sulfur dye and hydrochloric acid weak solution is put in the reactor that nickel alloy is made according to the amount that mass ratio is 1:0.54 and is stirred，Stirring reaction generates thiosulfuric acid and sodium chloride mixed solution in 2-3 hour，Carry out mixed solution being filtrated to get the most a small amount of filter cake impurity，Filter cake impurity is buried，The filtrate of clarification is sent in decompression distillator and carries out decompression distillation，Distillation time is 30-40 minute，Then crystallisation by cooling after heated distillation，The product obtained of cooling uses distilled water to carry out washing 2-3 time，Product after washing is dried 2-3 hour in exsiccator，Dried product carries out crushing packing and has obtained sodium chloride crystal product，Remaining distillating liquid is thiosulfuric acid weak solution semi-finished product，Thiosulfuric acid weak solution semi-finished product are placed in depurator，It is then placed in the silver hydroxide that mass fraction is 0.1%-0.5% and forms silver nitride precipitation，After filtration, remaining sodium hydroxide solution adds the calcium chloride of 0.3%-0.7% and is neutralized and obtains calcium hydroxide precipitation，Filter again，The most a small amount of remaining sodium chloride molecule after filtration，Then filtrate is carried out decompression distillation、Concentration finally obtains 75-85% thiosulfuric acid liquid.
The method have the advantages that its method is simple, discarded oxidation filtrate is re-used, prepare thiosulfuric acid and sodium chloride product; can effectively administer and make use of sulfur dye oxidation filtrate; not only protect environment, saved resource simultaneously, create good economic benefit.
Detailed description of the invention:
nullThis detailed description of the invention takes techniques below scheme: the oxidation filtrate of sulfur dye and hydrochloric acid weak solution is put in the reactor that nickel alloy is made according to the amount that mass ratio is 1:0.54 and is stirred，Stirring reaction generates thiosulfuric acid and sodium chloride mixed solution in 2-3 hour，Carry out mixed solution being filtrated to get the most a small amount of filter cake impurity，Filter cake impurity is buried，The filtrate of clarification is sent in decompression distillator and carries out decompression distillation，Distillation time is 30-40 minute，Then crystallisation by cooling after heated distillation，The product obtained of cooling uses distilled water to carry out washing 2-3 time，Product after washing is dried 2-3 hour in exsiccator，Dried product carries out crushing packing and has obtained sodium chloride crystal product，Remaining distillating liquid is thiosulfuric acid weak solution semi-finished product，Thiosulfuric acid weak solution semi-finished product are placed in depurator，It is then placed in the silver hydroxide that mass fraction is 0.1%-0.5% and forms silver nitride precipitation，After filtration, remaining sodium hydroxide solution adds the calcium chloride of 0.3%-0.7% and is neutralized and obtains calcium hydroxide precipitation，Filter again，The most a small amount of remaining sodium chloride molecule after filtration，Then filtrate is carried out decompression distillation、Concentration finally obtains 75-85% thiosulfuric acid liquid.
This detailed description of the invention has the advantages that its method is simple; discarded oxidation filtrate is re-used; prepare thiosulfuric acid and sodium chloride product; can effectively administer and make use of sulfur dye oxidation filtrate; not only protect environment; save resource simultaneously, create good economic benefit.
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 (1)
- null1. one kind uses the method that sulfur dye filtrate prepares thiosulfuric acid and sodium chloride，The preparation method that it is characterized in that it is: the oxidation filtrate of sulfur dye and hydrochloric acid weak solution is put in the reactor that nickel alloy is made according to the amount that mass ratio is 1:0.54 and is stirred，Stirring reaction generates thiosulfuric acid and sodium chloride mixed solution in 2-3 hour，Carry out mixed solution being filtrated to get the most a small amount of filter cake impurity，Filter cake impurity is buried，The filtrate of clarification is sent in decompression distillator and carries out decompression distillation，Distillation time is 30-40 minute，Then crystallisation by cooling after heated distillation，The product obtained of cooling uses distilled water to carry out washing 2-3 time，Product after washing is dried 2-3 hour in exsiccator，Dried product carries out crushing packing and has obtained sodium chloride crystal product，Remaining distillating liquid is thiosulfuric acid weak solution semi-finished product，Thiosulfuric acid weak solution semi-finished product are placed in depurator，It is then placed in the silver hydroxide that mass fraction is 0.1%-0.5% and forms silver nitride precipitation，After filtration, remaining sodium hydroxide solution adds the calcium chloride of 0.3%-0.7% and is neutralized and obtains calcium hydroxide precipitation，Filter again，The most a small amount of remaining sodium chloride molecule after filtration，Then filtrate is carried out decompression distillation、Concentration finally obtains 75-85% thiosulfuric acid liquid.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610150810.4A CN105819407A (en) | 2016-03-17 | 2016-03-17 | Method of preparing thiosulfuric acid and sodium chloride from filtrate of vulcanized dye |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610150810.4A CN105819407A (en) | 2016-03-17 | 2016-03-17 | Method of preparing thiosulfuric acid and sodium chloride from filtrate of vulcanized dye |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN105819407A true CN105819407A (en) | 2016-08-03 |
Family
ID=56523864
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610150810.4A Pending CN105819407A (en) | 2016-03-17 | 2016-03-17 | Method of preparing thiosulfuric acid and sodium chloride from filtrate of vulcanized dye |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN105819407A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106242186A (en) * | 2016-08-31 | 2016-12-21 | 浙江奇彩环境科技股份有限公司 | A kind of recycling processing method of sulphur black technique waste water |
-
2016
- 2016-03-17 CN CN201610150810.4A patent/CN105819407A/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 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106242186A (en) * | 2016-08-31 | 2016-12-21 | 浙江奇彩环境科技股份有限公司 | A kind of recycling processing method of sulphur black technique waste water |
| CN106242186B (en) * | 2016-08-31 | 2019-04-30 | 浙江奇彩环境科技股份有限公司 | A kind of recycling processing method of sulphur black technique waste water |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| WO2018041272A1 (en) | Method for preparing industrial grade lithium carbonate from crude lithium fluoride, and a lithium carbonate product | |
| CN101817989B (en) | Method for preparing disperse blue 60 and homologues thereof | |
| CN1843938A (en) | Method for preparing vanadium pentoxide | |
| CN104774165A (en) | Green and industrial preparation method of rubber peptizer DBD | |
| CN111484079B (en) | Method for preparing chromium oxide green from chromium-containing waste liquid in naphthoquinone production | |
| CN102303941B (en) | Deep dealkalizing method of red mud in alumina factory | |
| CN104016835B (en) | Sulfonation and alkali fusion optimized production process for 2- naphthol | |
| CN102923722A (en) | Preparation method for white carbon black | |
| CN102993026B (en) | Preparation method of p-phenylenediamine | |
| CN105858676A (en) | Production method for coproducing sodium silicate and sodium fluoride | |
| CN102367238A (en) | Method for synthesizing accelerator N,N-dicyclohexyl-2-benzothiazole sulfenamide | |
| CN105819407A (en) | Method of preparing thiosulfuric acid and sodium chloride from filtrate of vulcanized dye | |
| CN103073031A (en) | Method for preparing lithium fluoride from phosphate fertilizer by-product sodium fluoride | |
| CN103130196A (en) | Method for removing impurities from industrial sodium hydrosulfide | |
| CN111847518A (en) | Efficient recycling method of silicomanganese slag | |
| CN101633495A (en) | Method for preparing sulphur black dye and sodium thiosulfate from sulphur dye waste water | |
| CN103613685A (en) | Method for preparing chitin through subcritical hydrolysis of arthropod shells | |
| CN215975001U (en) | Water recycling system for preparing sulfuric acid method titanium dioxide calcining seed crystal | |
| CN111349015A (en) | Clean production process of monoamino anthraquinone | |
| CN105692565A (en) | Preparation method of calcium thiosualfate | |
| CN105883836A (en) | Co-production method of sodium metasilicate and sodium fluoride | |
| CN101774924B (en) | Production method of high-quality p-nitrophenol | |
| CN102944642B (en) | A kind of preparation method of iodine value reagent of improvement | |
| CN105523951A (en) | Synthetic method of 2-amino-N,3-dimethyl-4-chloro-5-bromobenzamide | |
| CN105600756A (en) | Preparation method of sodium thiosulfate |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20160803 |