CN104445090A - One step method for preparing anhydrous sodium sulfide through reduction of sodium sulfate by using carbon black or ultralow ash pure coal - Google Patents

One step method for preparing anhydrous sodium sulfide through reduction of sodium sulfate by using carbon black or ultralow ash pure coal Download PDF

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Publication number
CN104445090A
CN104445090A CN201310428231.8A CN201310428231A CN104445090A CN 104445090 A CN104445090 A CN 104445090A CN 201310428231 A CN201310428231 A CN 201310428231A CN 104445090 A CN104445090 A CN 104445090A
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sodium sulfide
carbon black
sodium
content
reaction
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CN104445090B (en
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许涛
赵秀平
荆小兵
苏刚
于惠霞
高秀云
李胜
武向前
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Nanfeng Chemical (Yuncheng) Group Co.,Ltd.
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NANFENG CHEMICAL GROUP CO Ltd
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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
    • C01B17/22—Alkali metal sulfides or polysulfides
    • C01B17/24—Preparation by reduction
    • C01B17/26—Preparation by reduction with carbon

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Treating Waste Gases (AREA)
  • Solid-Sorbent Or Filter-Aiding Compositions (AREA)
  • Pigments, Carbon Blacks, Or Wood Stains (AREA)
  • Processing Of Solid Wastes (AREA)

Abstract

The invention relates to a novel method for preparing anhydrous sodium sulfide in one step. Carbon black or ultralow ash pure coal is used as a reductant for the first time and reacted with sodium sulfate to produce anhydrous sodium sulfide with the content more than 90% in one step. To prevent sodium sulfide from being oxidated and from reactor material corrosion under a condition with a high sodium sulfide content and a high temperature, the reaction is carried out in a self-made reactor made of special material under the protection of inert gases. The process has the following advantages that: firstly, the product can be obtained in one step with pure raw materials in a special reacting condition and a series of subsequent processes such as solution leaching, settling, separating, evaporating and the like in the present process of sodium sulfide production can be avoided, and the technological process is shortened, especially the evaporating process is omitted, and the energy consumption is greatly saved; secondly, there is largely no waste water, waste slag and waste gas discharged in the whole productive process; thirdly, the obtained product has a high sodium sulfide content and increased additional value and can be widely used. According to the invention, the present situation that the traditional productive process of sodium sulfide is tedious and has high energy consumption and severe pollution for years will be thoroughly changed by implementing the process. The process in the invention is energy efficient and environment-friendly, and meets the need of modern production strategy, and has significant economic benefits and social benefits. Furthermore, there is no related research reported at home and abroad at present.

Description

Carbon black or ultra low-ash pure coal reduction sodium sulfate single stage method prepare the method for Sodium sulphate anhydrous, 99min
Technical field
The present invention relates to a kind of novel method preparing Sodium sulphate anhydrous, 99min, especially relating to one carbon black or ultra low-ash pure coal is reductive agent and sodium sulfate reaction, and by creating special reaction conditions, single stage method can obtain the novel process of Sodium sulphate anhydrous, 99min finished product.
Background technology
The production of current domestic sodium sulphite mainly obtains " grey black " with common ash coal reduction sodium sulfate, and then finally obtains by molten leaching, sedimentation, evaporation, film-making etc. series of processes the sodium sulphite that content is 60%.Due to the restriction by raw material and technology, there is following problem in this production technique:
(1) complex technical process is tediously long, troublesome poeration, and labour intensity is large;
(2) all need to consume a large amount of fire coals at calcination reaction and evaporative process, energy consumption is high;
(3) whole production process is polluted very serious, and the discharge of a large amount of sulphur-containing exhaust gas, waste water and waste residue creates to nearby residents life and ecotope and has a strong impact on, and is difficult to thorough solution for many years.
(4) products obtained therefrom sodium sulfide content is generally about 60%, and content is low, and kind is single.And in recent years along with the development of some high-tech areas, more and more higher to the requirement that becomes more meticulous of sodium sulphite product, currently available products can not be met the need of market far away.
In the face of the sodium sulphite of this high energy consumption, high pollution is produced, reduce discharging the strong request of situation at present at national energy-saving under, the Sodium Sulphide enterprise of domestic more than 95% is all listed among environmental protection " Black List ", the crisis of be faced with stopping production, changing the line of production.
In order to Sustainable development, change the backward Sodium Sulphide production technique of existing tradition and technology, the present invention proposes with pure carbon black or ultra low-ash pure coal (coal of the solid carbon of low ash height) as reductive agent, react with the industrial sulphuric acid sodium of 99%, and go out the Sodium sulphate anhydrous, 99min product of content more than 90% by measure One-step productions such as Controlling Technology conditions, thus eliminate the sequence of operations of follow-up (comprise molten leaching, sedimentation, wash mud, evaporation etc.), whole technical process is shortened dramatically, energy consumption reduces, three-waste free discharge.And the raising of product sodium sulfide content can not only be saved packing cost and be slowed down transport pressure, this high-content sodium sulphite of what is more important can also be applied to other high-tech area, such as the synthesis etc. of high-grade engineering plastics polyphenylene sulfide (being called for short PPS resin), added value of product is greatly increased.All drawbacks that this invented technology overcomes existing sodium sulphite and produces can be said, no matter at home or abroad, to the production technology progress of sodium sulphite, all there is epoch-making meaning.Up to the present, an enterprise or research institution is not had to carry out research report to this sodium sulphite Technology both at home and abroad.
Meanwhile, for the preparation of Sodium sulphate anhydrous, 99min product, domestic and international currently used method is all use moisture sodium sulphite, such as Na 2s.9H 2o, Na 2s.5.5H 2o, Na 2s.3H 2o etc. are through vacuum dehydration or add dehydration of organic solvent and obtain, and these technology are known.Such as EP-B-0345 136, EP-B-0361 998, P00116141.5 etc., but their production prerequisite all needs first to obtain moisture sodium sulphite is used as dry raw material, so fundamentally still do not escape the production technique category of existing sodium sulphite, and small scale, to yield poorly.In addition, in generation twentieth century 30 or 40 years, gas (H was once in the Soviet Union, Germany, Japan, China etc. 2, CO, Sweet natural gas etc.) reduction sodium sulfate produces the large quantity research report of Sodium sulphate anhydrous, 99min, but glue wall or add the various problems such as catalyzer finally could not realize industrialization because there is material.
Summary of the invention
The object of this invention is to provide a kind of not only can effectively to overcome at present traditional with common coal for the defect of severe contamination that sodium sulphite causes environment and high energy consumption to be produced by reductive agent through series of processes, and the product preparation process of sodium sulfide content more than 90% can be obtained.It utilizes carbon black or ultra low-ash pure coal to be raw material, and the reaction of industrial sulphuric acid sodium, and by selecting and creating the Sodium sulphate anhydrous, 99min that special reaction conditions single stage method obtains high-content.
The present invention is implemented by following technical scheme: this preparation method includes following steps:
1) carbon black or particle diameter are pressed Na at the ultra low-ash pure coal of below 0.1mm and industrial sulphuric acid sodium 2sO 4: the equimolar ratio batching of 2C=1:1, fully mixing is placed in the atmosphere protection reduction furnace made with exotic materials.
2) pass into after the inertia protection air-blowing air swept in stove is about 30min, by certain temperature rise rate temperature programming, about 823 DEG C time, reaction starts, and continues be warming up to 1150 DEG C and be incubated 40min, the CO of reaction process protection gas and generation 2gas is protected to return recycle after tail gas alkali liquor absorption.
3) under atmosphere protection condition, open discharge system and carry out discharging, carry out shaping and packaging after slightly cold, obtain sodium sulphite finished product, block in loose honeycomb.
Adopt carbon black or ultra low-ash pure coal to be the water-insoluble that reductive agent can ensure lower aq in product, in general warranty coal, ash content is even lower below 3%, then in product water-insoluble below 1.0%; When requiring the product obtaining lower water-insoluble then selection carbon black as reductive agent; When using carbon black, wherein carbon containing>=97%; When using ultra low-ash pure coal, ash content≤3% wherein, fixed carbon>=88%; Sodium sulfate adopts the regulation of GB 6009-2003 industrial sulphuric acid sodium I class acceptable end product or premium grads, Na 2sO 4>=99%.
Material carbon and sodium sulfate are prepared burden in strict accordance with equimolar ratio and are reacted, otherwise unnecessary raw material will remain and becomes impurity in the product, and especially excessive carbon existence can cause the raising of water insoluble matter content in product and affect product appearance.Such mole batching such as grade also makes the amount ratio of reduction coal existing production reduction coal consumption reduce about 40% simultaneously;
React in atmosphere of inert gases, efficiently avoid because of O in air 2, H 2the existence of O etc. and a series of side reactions occurred, thus ensured the raising of the main content of sodium sulphite.Preferred nitrogen;
Adopt special substance to make reactor linings, it can the at high temperature corrosion of resistance to sodium sulphite and seepage well, thus ensure that carrying out smoothly and the impurity effect that produces because of material corrosion in product of reaction;
Reaction, about 823 DEG C of beginnings, peaks when 920 DEG C, is warming up to 1150 DEG C and can ensures that reaction can be carried out thoroughly, being also convenient to discharging;
Experiment proves that this reaction is within very short time, generally can complete in 20 min, and material increases the reaction time can proper extension;
Reaction terminate after when atmosphere protection bottom discharge can reduce high temperature the aerial oxidation of sodium sulphite and deliquescence;
Product appearance is red or light red, loose cellular;
Sodium sulfide content is 90%, and generally more than 92%, and 60% current sodium sulphite product compares, and not only can save packing cost, slow down transport pressure, this anhydrous product is not oxidizable yet simultaneously, so it has excellent accumulating performance.
The invention has the advantages that: it use purer reductive agent on the one hand, carbon black or ultra low-ash pure coal, on the other hand again by creating the conditions such as the reactor of inert reaction atmosphere and employing exotic materials, fundamentally overcome all issuable side reactions of reduction process and avoid the impurity effect that raw material and reactor material produce product, single stage method obtains comparatively pure product, no longer need follow-up treating processes, flow process is short, energy consumption is low, three-waste free discharge, packaging and transportation cost have not only been saved in the raising of sodium sulfide content, and its Application Areas is also wider, such as, the synthesis etc. of high-grade engineering plastics polyphenylene sulfide can be advantageously applied to, profit is higher.
accompanying drawing illustrates:
Fig. 1 is that the present invention prepares Sodium sulphate anhydrous, 99min process flow sheet, and Fig. 2 is current production technology of sodium sulfide schema.
embodiment:
embodiment 1: carbon black single stage method reduction sodium sulfate prepares the method for anhydrous high-content sodium sulphite, and to produce 1 Kg Sodium sulphate anhydrous, 99min for benchmark, this preparation method includes following steps:
1) 0.317Kg carbon black is fully mixed with 1.84Kg industrial sulphuric acid sodium be placed in homemade special reaction stove.
2) after the air passed in nitrogen purging stove is about 30min, start program heats up, simultaneously with 0.3m 3the flow of/h continues to pass into nitrogen.About 823 DEG C time, reaction starts, and continues to heat up, is incubated 40min again, then stopped reaction when temperature reaches 1150 DEG C.
3) under atmosphere protection condition, discharge system discharging is opened, slightly cold aftershaping, packaging.Gained sodium sulphite is that light red is loosened honeycomb bulk, analyzes its sodium sulfide content 94.2%, water-insoluble 0.10%.
embodiment 2:ultra low-ash pure coal single stage method reduction sodium sulfate prepares the method for anhydrous high-content sodium sulphite, and to produce 1 Kg Sodium sulphate anhydrous, 99min for benchmark, this preparation method includes following steps:
1) 0.350Kg ultra low-ash pure coal is fully mixed with 1.84Kg industrial sulphuric acid sodium be placed in homemade special Reaktionsofen.
2) after the air passed in nitrogen purging stove is about 30min, start program heats up, simultaneously with 0.3m 3the flow of/h continues to pass into nitrogen.About 823 DEG C time, reaction starts, and continues to heat up, is incubated 40min again, then stopped reaction when temperature reaches 1150 DEG C.
3) under atmosphere protection condition, discharge system discharging is opened, slightly cold aftershaping, packaging.Gained sodium sulphite is that red loose honeycomb is block, analyzes its sodium sulfide content 92.8%, water-insoluble 0.68%.
embodiment 3:ultra low-ash pure coal single stage method reduction sodium sulfate prepares the method for anhydrous high-content sodium sulphite, and to produce 10 Kg Sodium sulphate anhydrous, 99mins for benchmark, this preparation method includes following steps:
1) 3.50Kg ultra low-ash pure coal is fully mixed with 18.4Kg industrial sulphuric acid sodium be placed in homemade special Reaktionsofen.
2) after the air passed in nitrogen purging stove is about 30min, start program heats up, simultaneously with 0.3m 3the flow of/h continues to pass into nitrogen.About 823 DEG C time, reaction starts, and continues to heat up, is incubated 40min again, then stopped reaction when temperature reaches 1150 DEG C.
3) under atmosphere protection condition, discharge system discharging is opened, slightly cold aftershaping, packaging.
Gained sodium sulphite is that red loose honeycomb is block, analyzes that its sodium sulfide content is 93.4%, water-insoluble is 0.61%.
In embodiment carbon black used, fixed carbon is 99.0%; Fixed carbon 89.9%, ash content 2.19% in ultra low-ash pure coal used.

Claims (7)

1. carbon black or ultra low-ash pure coal reduction sodium sulfate single stage method prepare sodium sulphite that is anhydrous, high-content; it is characterized in that; the carbon black of certain particle size or ultra low-ash pure coal and sodium sulfate are fully mixed by certain ratio of components; be placed in the high-temperature reactor that exotic materials makes; after passing into protection gas; control certain temperature rise rate be heated to temperature required after react, reaction terminate after under atmosphere protection, carry out discharging, the product that sodium sulfide content is more than 90% can be obtained.
2. method according to claim 1, is characterized in that reductive agent used is carbon black or ultra low-ash pure coal, and carbon black reduction products obtained therefrom is more pure, and water-insoluble is lower.
3. method according to claim 1, when it is characterized in that using carbon black, wherein carbon containing>=97%; When using ultra low-ash pure coal, ash content≤3% wherein, fixed carbon>=88%; Sodium sulfate adopts the regulation of GB 6009-2003 industrial sulphuric acid sodium I class acceptable end product or premium grads, Na 2sO 4>=99%.
4. method according to claim 1, is characterized in that reactor used is that homemade exotic materials makes, can fire resistant anticorrosive antiseep.
5. method according to claim 1, it is characterized in that reacting is carry out in the atmosphere of protection of inert gas, and first-selection is nitrogen.
6. method according to claim 1, adopts equimolar ratio batching, i.e. Na when it is characterized in that reaction 2sO 4: 2C=1:1; Temperature of reaction is 823 DEG C ~ 1150 DEG C, reaction times 40 ~ 60min, starts discharge system discharging after reaction terminates under atmosphere protection condition.
7., according to the method for claim 1-6, it is characterized in that the sodium sulphite of preparation is for red loose honeycomb bulk, divides two kinds: carbon black products obtained therefrom sodium sulfide content is generally more than 94%, and water-insoluble is below 0.2%; Ultra low-ash pure coal products obtained therefrom outward appearance takes on a red color, and sodium sulfide content is generally more than 92%, water-insoluble less than 1.0%.
CN201310428231.8A 2013-09-22 2013-09-22 The method that carbon black or ultra low-ash pure coal reduction sodium sulphate one-step method prepare anhydrous sodium sulfide Active CN104445090B (en)

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107619025A (en) * 2016-07-13 2018-01-23 南风化工集团股份有限公司 A kind of gas reduction sodium sulphate prepares the new technology of anhydrous sodium sulfide
CN112985064A (en) * 2021-02-05 2021-06-18 陕西翼飞航智能科技有限公司 Sintering device and sintering method based on plasma hot blast stove
CN113007895A (en) * 2021-02-05 2021-06-22 陕西翼飞航智能科技有限公司 Based on CO2Sodium sulfide production and CO production in plasma hot blast stove2Recovery system and method
WO2024040703A1 (en) * 2022-08-24 2024-02-29 湖南福尔程环保科技有限公司 Resource utilization method for crude sodium sulfate

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US1540711A (en) * 1922-08-03 1925-06-02 Merrimac Chemical Co Process for the manufacture of sodium sulphide
US1584597A (en) * 1925-08-26 1926-05-11 Harry P Bassett Process of making sodium sulphide
CN1056662A (en) * 1991-07-17 1991-12-04 王思翔 Alkali sulfide produced by activated method
CN1244493A (en) * 1999-09-13 2000-02-16 甘肃亚盛盐化工业集团有限责任公司 Production technology of yellow flaky sodium sulfide with low carbon and iron contents
CN101565173A (en) * 2009-05-31 2009-10-28 孔凡逸 Semi-vertical reverberatory furnace for preparing sodium sulfide and process thereof
CN101585512A (en) * 2009-06-18 2009-11-25 赵志军 Method of producing anhydrous sodium sulfide without pollution
CN101948100A (en) * 2010-10-08 2011-01-19 赵志军 Clean method for producing anhydrous sodium sulfide

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US1540711A (en) * 1922-08-03 1925-06-02 Merrimac Chemical Co Process for the manufacture of sodium sulphide
US1584597A (en) * 1925-08-26 1926-05-11 Harry P Bassett Process of making sodium sulphide
CN1056662A (en) * 1991-07-17 1991-12-04 王思翔 Alkali sulfide produced by activated method
CN1244493A (en) * 1999-09-13 2000-02-16 甘肃亚盛盐化工业集团有限责任公司 Production technology of yellow flaky sodium sulfide with low carbon and iron contents
CN101565173A (en) * 2009-05-31 2009-10-28 孔凡逸 Semi-vertical reverberatory furnace for preparing sodium sulfide and process thereof
CN101585512A (en) * 2009-06-18 2009-11-25 赵志军 Method of producing anhydrous sodium sulfide without pollution
CN101948100A (en) * 2010-10-08 2011-01-19 赵志军 Clean method for producing anhydrous sodium sulfide

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107619025A (en) * 2016-07-13 2018-01-23 南风化工集团股份有限公司 A kind of gas reduction sodium sulphate prepares the new technology of anhydrous sodium sulfide
CN112985064A (en) * 2021-02-05 2021-06-18 陕西翼飞航智能科技有限公司 Sintering device and sintering method based on plasma hot blast stove
CN113007895A (en) * 2021-02-05 2021-06-22 陕西翼飞航智能科技有限公司 Based on CO2Sodium sulfide production and CO production in plasma hot blast stove2Recovery system and method
WO2024040703A1 (en) * 2022-08-24 2024-02-29 湖南福尔程环保科技有限公司 Resource utilization method for crude sodium sulfate

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