CN101823730A - Method for simultaneously producing sodium thiocyanate and ammonium carbonate - Google Patents
Method for simultaneously producing sodium thiocyanate and ammonium carbonate Download PDFInfo
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- CN101823730A CN101823730A CN 201010185180 CN201010185180A CN101823730A CN 101823730 A CN101823730 A CN 101823730A CN 201010185180 CN201010185180 CN 201010185180 CN 201010185180 A CN201010185180 A CN 201010185180A CN 101823730 A CN101823730 A CN 101823730A
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Abstract
本发明涉及以从焦化厂脱硫废液中回收的粗硫氰酸钠为原料，同时生产硫氰酸钠和碳酸铵的方法，其特征为：取粗硫氰酸铵加入与硫氰酸铵等物质的量的碳酸氢钠混合，或加入1/2硫氰酸铵的物质的量的碳酸钠混合，再加入与粗硫氰酸铵等质量的水，加热并保持温度80-95℃，不搅拌或或5-300转/分钟低速搅拌，反应系统蒸汽逸出并引入冷凝器中析出碳酸铵晶体，反应进行4-20小时至反应液澄清透明，无气泡生成为止，反应液过滤后加硫酸至pH＝2-4，搅拌5-20分钟，再加入与粗硫氰酸铵中杂质等质量的氢氧化钙搅拌10-30分钟，过滤，滤液蒸发结晶得到硫氰酸钠产品。本发明生产工艺简单，所需投资较少，经济效益和社会效益都十分显著。The invention relates to a method for simultaneously producing sodium thiocyanate and ammonium carbonate using crude sodium thiocyanate recovered from the desulfurization waste liquid of a coking plant as a raw material. Mix the amount of sodium bicarbonate with the amount of substance, or add 1/2 the amount of sodium carbonate with the amount of ammonium thiocyanate, then add water equal to the quality of crude ammonium thiocyanate, heat and keep the temperature at 80-95°C, do not Stir or stir at a low speed of 5-300 rpm, the steam in the reaction system escapes and is introduced into the condenser to precipitate ammonium carbonate crystals, and the reaction is carried out for 4-20 hours until the reaction liquid is clear and transparent, and no bubbles are formed. After the reaction liquid is filtered, add sulfuric acid To pH = 2-4, stirring for 5-20 minutes, then adding calcium hydroxide of the same mass as the impurities in the crude ammonium thiocyanate, stirring for 10-30 minutes, filtering, evaporating and crystallizing the filtrate to obtain sodium thiocyanate product. The production process of the invention is simple, the required investment is less, and the economic and social benefits are very remarkable.
Description
Technical field
The invention belongs to chemical production field, being specifically related to a kind of is raw material with the thick ammonium thiocyanate that contains more impurity that coking desulfurization waste liquor was extracted, and produces the method for Sodium Thiocyanate 99 and volatile salt simultaneously.
Background technology
At present, domestic many coke-oven plants adopt the HPF desulfurization and decyanation technology, and this technology must efflux a part of desulfurization waste liquor and keep the skin wet to keep higher desulfuration efficiency.Containing a large amount of ammonium thiocyanates, ammonium thiosulfate, ammonium sulphite and ammonium sulfate etc. in the desulfurization waste liquor, is the complex mixture of multiple toxic substance.The coke-oven plant does not all have treatment process preferably to this desulfurization waste liquor at present, generally adopts to be sprayed onto on the coal yard, mixes in the coking coal.Such result has not only increased the energy consumption of process of coking, and severe contamination underground water.Another aspect, the thiocyanate concn in the desulfurization waste liquor is big, and the content height is the very high Chemicals of added value.From efflux desulfurization waste liquor, reclaim thiocyanate-, not only can the regenerative sulfur binding waste liquid, and remarkable in economical benefits, be the practicable method of recycling treatment desulfurization waste liquor.
Patent CN101125644A adopts the vacuum distilling method to extract ammonium thiosulfate and ammonium thiocyanate product respectively from coking desulfurization waste liquor, these class methods are the main method of domestic processing coking desulfurization waste liquor at present, but the ammonium thiocyanate product purity that obtains is lower, content is about 60-95%, thereby purposes is limited, and economic benefit is also not so good.The thick ammonium thiocyanate that this class is extracted from coking desulfurization waste liquor carries out purifying, conversion processing, has not only increased economic benefit, has also promoted vacuum distilling to handle the popularization of coking desulfurization waste liquor technology.
Summary of the invention
The thick ammonium thiocyanate that this patent is lower with the purity of being extracted from coking desulfurization waste liquor, foreign matter content is more is a raw material, produces purity greater than 96% Sodium Thiocyanate 99 by conversion processing, produces purity simultaneously greater than 98% volatile salt product.
Concrete steps of the present invention comprise:: get the thick ammonium thiocyanate that contains more impurity that coking desulfurization waste liquor extracts and add with the sodium bicarbonate of amount of substance such as ammonium thiocyanate and mix, or the yellow soda ash that adds the amount of substance of 1/2 ammonium thiocyanate mixes, add water again with quality such as thick ammonium thiocyanate, heating also keeps 80-95 ℃ of temperature, do not stir or 5-300 rev/min of stirring at low speed, reactive system steam is overflowed and is introduced in the condenser and separate out the volatile salt crystal, reaction is carried out 4-20 hour to the reaction solution clear, till no bubble generates, the acid of reacting liquid filtering after vulcanization is to pH=2-4, stirred 5-20 minute, add again with thick ammonium thiocyanate in the calcium hydroxide of quality such as impurity stirred 10-30 minute, filter, the filtrate evaporative crystallization obtains the Sodium Thiocyanate 99 product.
The described method production technique of this patent is simple, and required investment is less, and economic benefit and social benefit are all very remarkable.
Embodiment
Example 1
The purity of extracting from coking desulfurization waste liquor that getting Yangzhou Kang Long Ingegneria Ambientale SRL is provided is 94% thick ammonium thiocyanate 100 grams, adding anhydrous sodium carbonate 66 grams mixes, add 100 milliliters of entry again, heating also keeps 80-85 ℃ of temperature, do not stir, the spontaneous effusion of reactive system steam is also introduced in the condenser and is separated out the volatile salt crystal, reaction is carried out 20 hours to the reaction solution clear, till no bubble generates, the acid of reacting liquid filtering after vulcanization was stirred 5 minutes to pH=2, added calcium hydroxide 6 grams again and stirred 30 minutes, filter, the filtrate evaporative crystallization obtains the Sodium Thiocyanate 99 product.According to chemical industry standard HG/T 3812-2006 the Sodium Thiocyanate 99 product is tested, the Sodium Thiocyanate 99 product purity is 98%, reaches industrial acceptable end product standard.The volatile salt assay is that purity is greater than 99%.
Example 2
The purity of extracting from coking desulfurization waste liquor that getting Yangzhou Kang Long Ingegneria Ambientale SRL is provided is 94% thick ammonium thiocyanate 100 grams, adding and manually synthesizing purity after ammonium sulfate 50 grams mix is 62.67% thick ammonium thiocyanate 150 grams, adding sodium bicarbonate 104 grams mixes, add 150 milliliters of entry again, heating also keeps 90-95 ℃ of temperature, keep 300 rev/mins of stirrings, introduce in the condenser after reactive system steam is overflowed and separate out the volatile salt crystal, reaction is carried out 4 hours to the reaction solution clear, till no bubble generates, the acid of reacting liquid filtering after vulcanization is to pH=4, stirred 20 minutes, add calcium hydroxide 50 grams again and stirred 10 minutes, filter, the filtrate evaporative crystallization obtains the Sodium Thiocyanate 99 product.According to chemical industry standard HG/T 3812-2006 the Sodium Thiocyanate 99 product is tested, the Sodium Thiocyanate 99 product purity is 96%, reaches industrial salable product standard.The volatile salt assay is that purity is greater than 98%.
Claims (3)
1. method of producing Sodium Thiocyanate 99 and volatile salt simultaneously, its step is as follows: get thick ammonium thiocyanate and add with the sodium bicarbonate of amount of substance such as ammonium thiocyanate and mix, or the yellow soda ash that adds the amount of substance of 1/2 ammonium thiocyanate mixes, add water again with quality such as thick ammonium thiocyanate, heating also keeps 80-95 ℃ of temperature, do not stir or stirring at low speed, separate out the volatile salt crystal in steam effusion and the introducing condenser in the reactive system, reaction is carried out 4-20 hour to the reaction solution clear, till no bubble generates, the acid of reacting liquid filtering after vulcanization is to pH=2-4, stirred 5-20 minute, add again with thick ammonium thiocyanate in the calcium hydroxide of quality such as impurity stirred 10-30 minute, filter, the filtrate evaporative crystallization obtains the Sodium Thiocyanate 99 product.
2. require in 1 described a kind of step of producing Sodium Thiocyanate 99 and volatile salt simultaneously according to letter of authorization, used thick ammonium thiocyanate is the ammonium thiocyanate that contains more impurity that coking desulfurization waste liquor extracted.
3. require in 1 described a kind of step of producing Sodium Thiocyanate 99 and volatile salt simultaneously according to letter of authorization, stirring at low speed refers to 5-300 rev/min stirring.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN 201010185180 CN101823730A (en) | 2010-05-25 | 2010-05-25 | Method for simultaneously producing sodium thiocyanate and ammonium carbonate |
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| Application Number | Priority Date | Filing Date | Title |
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| CN 201010185180 CN101823730A (en) | 2010-05-25 | 2010-05-25 | Method for simultaneously producing sodium thiocyanate and ammonium carbonate |
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| CN101823730A true CN101823730A (en) | 2010-09-08 |
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| CN 201010185180 Pending CN101823730A (en) | 2010-05-25 | 2010-05-25 | Method for simultaneously producing sodium thiocyanate and ammonium carbonate |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104925830A (en) * | 2015-07-10 | 2015-09-23 | 安徽工业大学 | Chemical treatment method for extracting sodium thiocyanate from coked desulfurization waste solution |
| CN106006674A (en) * | 2016-05-23 | 2016-10-12 | 定州旭阳科技有限公司 | Method for simultaneously preparing potassium thiocyanate, potassium sulfate and ammonium carbonate from desulfurization waste solution |
| CN112340911A (en) * | 2020-09-29 | 2021-02-09 | 陕西陕焦化工有限公司 | Method for recycling desulfurization waste liquid |
| CN112340912A (en) * | 2020-09-29 | 2021-02-09 | 陕西陕焦化工有限公司 | Method for recovering inorganic salt in ammonia desulphurization waste liquid |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1034349A (en) * | 1988-01-21 | 1989-08-02 | 化学工业部上海化工研究院 | The recovery method of ammonium thiocyanate |
| JPH01219049A (en) * | 1988-02-26 | 1989-09-01 | Sumikin Chem Co Ltd | Additive for cement and its production |
| JP2550575B2 (en) * | 1987-05-11 | 1996-11-06 | 住金化工株式会社 | Recovery method of ammonium thiocyanate |
-
2010
- 2010-05-25 CN CN 201010185180 patent/CN101823730A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2550575B2 (en) * | 1987-05-11 | 1996-11-06 | 住金化工株式会社 | Recovery method of ammonium thiocyanate |
| CN1034349A (en) * | 1988-01-21 | 1989-08-02 | 化学工业部上海化工研究院 | The recovery method of ammonium thiocyanate |
| JPH01219049A (en) * | 1988-02-26 | 1989-09-01 | Sumikin Chem Co Ltd | Additive for cement and its production |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104925830A (en) * | 2015-07-10 | 2015-09-23 | 安徽工业大学 | Chemical treatment method for extracting sodium thiocyanate from coked desulfurization waste solution |
| CN104925830B (en) * | 2015-07-10 | 2016-10-05 | 安徽工业大学 | A chemical treatment method for extracting sodium thiocyanate from coking desulfurization waste liquid |
| CN106006674A (en) * | 2016-05-23 | 2016-10-12 | 定州旭阳科技有限公司 | Method for simultaneously preparing potassium thiocyanate, potassium sulfate and ammonium carbonate from desulfurization waste solution |
| CN106006674B (en) * | 2016-05-23 | 2017-11-21 | 定州旭阳科技有限公司 | The method for producing potassium rhodanide, potassium sulfate and ammonium carbonate simultaneously with desulfurization waste liquor |
| CN112340911A (en) * | 2020-09-29 | 2021-02-09 | 陕西陕焦化工有限公司 | Method for recycling desulfurization waste liquid |
| CN112340912A (en) * | 2020-09-29 | 2021-02-09 | 陕西陕焦化工有限公司 | Method for recovering inorganic salt in ammonia desulphurization waste liquid |
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